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2011 Volume 22 Issue 11
2011, 22(11): 1261-1264
doi: 10.1016/j.cclet.2011.07.002
Abstract:
4-and 6-desphenyl analogues of (-)-clausenamide, 6 and 7, were prepared in optical active form from commercially available D-pyroglutamic acid and the known racemic pyrrolidinone 13, respectively. In order to confirm the absolute stereochemistry of (+)-and (-)-7, intermediate 19b was transferred into the (+)-epi-clausenamide 8.
4-and 6-desphenyl analogues of (-)-clausenamide, 6 and 7, were prepared in optical active form from commercially available D-pyroglutamic acid and the known racemic pyrrolidinone 13, respectively. In order to confirm the absolute stereochemistry of (+)-and (-)-7, intermediate 19b was transferred into the (+)-epi-clausenamide 8.
2011, 22(11): 1265-1268
doi: 10.1016/j.cclet.2011.07.015
Abstract:
A series of C2-symmetric and asymmetric chiral thiourea derivatives were synthesized from commercial L-phenylalanine. All of the new compounds have been fully characterized by IR, 1H NMR, 13C NMR, MS spectra and elemental analyses. The chiral thioureas were used as chiral ligands in the catalytic enantioselective ethylation of aldehydes with diethylzinc, the corresponding sec-alcohols were gained with excellent enantioselectivities (up to 87.1% ee) and high yields (up to 76.7%) after the conditions were optimized.
A series of C2-symmetric and asymmetric chiral thiourea derivatives were synthesized from commercial L-phenylalanine. All of the new compounds have been fully characterized by IR, 1H NMR, 13C NMR, MS spectra and elemental analyses. The chiral thioureas were used as chiral ligands in the catalytic enantioselective ethylation of aldehydes with diethylzinc, the corresponding sec-alcohols were gained with excellent enantioselectivities (up to 87.1% ee) and high yields (up to 76.7%) after the conditions were optimized.
2011, 22(11): 1269-1272
doi: 10.1016/j.cclet.2011.05.033
Abstract:
Novel chiral PN4-type multidentate aminophosphine ligands have been successfully synthesized by Schiff-base condensation of bis(o-formylphenyl)phenylphosphane and various chiral amino-sulfonamides. Their structures were fully characterized by IR, EI-MS and NMR. The catalytic systems, prepared in situ from the multidentate ligands and iridium(I) complexes, showed high activity in asymmetric transfer hydrogenation of propiophenone in 2-propanol solution, leading to corresponding optical alcohol with up to 75% ee.
Novel chiral PN4-type multidentate aminophosphine ligands have been successfully synthesized by Schiff-base condensation of bis(o-formylphenyl)phenylphosphane and various chiral amino-sulfonamides. Their structures were fully characterized by IR, EI-MS and NMR. The catalytic systems, prepared in situ from the multidentate ligands and iridium(I) complexes, showed high activity in asymmetric transfer hydrogenation of propiophenone in 2-propanol solution, leading to corresponding optical alcohol with up to 75% ee.
2011, 22(11): 1273-1276
doi: 10.1016/j.cclet.2011.05.027
Abstract:
A mild and efficient method for preparation of novel 2, 2-dichloro-1, 3-diarylaziridines from Schiff base compounds in the presence of N-cetyl-N, N, N-trimethyl ammonium bromide (CTAB) as phase transfer catalyst has been described. The reaction is dramatically enhanced in the presence of quaternary ammonium salt. The corresponding products have been obtained in excellent yields, high purity and short reaction times.
A mild and efficient method for preparation of novel 2, 2-dichloro-1, 3-diarylaziridines from Schiff base compounds in the presence of N-cetyl-N, N, N-trimethyl ammonium bromide (CTAB) as phase transfer catalyst has been described. The reaction is dramatically enhanced in the presence of quaternary ammonium salt. The corresponding products have been obtained in excellent yields, high purity and short reaction times.
2011, 22(11): 1277-1280
doi: 10.1016/j.cclet.2011.05.030
Abstract:
A series of 2, 5-disubstituted pyrimido[5, 4-c]quinoline derivatives were synthesized and their cytotoxic activity against H460, HT-29 and MDA-MB-231 cell lines was evaluated in vitro. It was found that most of the tested compounds especially compound 17, shown stronger activity to the selected three cell lines than ZM447439.
A series of 2, 5-disubstituted pyrimido[5, 4-c]quinoline derivatives were synthesized and their cytotoxic activity against H460, HT-29 and MDA-MB-231 cell lines was evaluated in vitro. It was found that most of the tested compounds especially compound 17, shown stronger activity to the selected three cell lines than ZM447439.
2011, 22(11): 1281-1284
doi: 10.1016/j.cclet.2011.05.035
Abstract:
1, 10-Phenanthrolinium N-ylides, can react with malonitrile and aromatic aldehydes via a domino-Knoevenagel cyclization to afford a new class of mhydropyrrolo[l, 2-a] [l, 10]phenanthroline derivatives as stable helical compounds in a simple, mild, and efficient protocol in excellent yields.
1, 10-Phenanthrolinium N-ylides, can react with malonitrile and aromatic aldehydes via a domino-Knoevenagel cyclization to afford a new class of mhydropyrrolo[l, 2-a] [l, 10]phenanthroline derivatives as stable helical compounds in a simple, mild, and efficient protocol in excellent yields.
2011, 22(11): 1285-1288
doi: 10.1016/j.cclet.2011.06.016
Abstract:
A novel enantiopure salen ligand bearing a diphenylphosphine oxide on the 3-position of one aromatic ring was synthesized and combined with Ti(Oi-Pr)4 as a monometallic bifunctional catalyst for asymmetric cyanosilylation reaction of aldehydes with trimethylsilyl cyanide (TMSCN). The catalyst system exhibited excellent activity and moderate enantioselectivity. The addition of TMSCN to 4-nitrobenzaldehyde in the presence of 1 mol% catalyst loading could complete within 10 min at ambient temperature. An intramolecularly cooperative catalysis was observed in this system wherein the central metal Ti(IV) is suggested to play a role of Lewis acid to activate aldehydes while the appended diphenylphosphine oxide worked as Lewis base to activate TMSCN.
A novel enantiopure salen ligand bearing a diphenylphosphine oxide on the 3-position of one aromatic ring was synthesized and combined with Ti(Oi-Pr)4 as a monometallic bifunctional catalyst for asymmetric cyanosilylation reaction of aldehydes with trimethylsilyl cyanide (TMSCN). The catalyst system exhibited excellent activity and moderate enantioselectivity. The addition of TMSCN to 4-nitrobenzaldehyde in the presence of 1 mol% catalyst loading could complete within 10 min at ambient temperature. An intramolecularly cooperative catalysis was observed in this system wherein the central metal Ti(IV) is suggested to play a role of Lewis acid to activate aldehydes while the appended diphenylphosphine oxide worked as Lewis base to activate TMSCN.
Synthesis of vegetable oil based polyol with cottonseed oil and sorbitol derived from natural source
2011, 22(11): 1289-1292
doi: 10.1016/j.cclet.2011.05.043
Abstract:
In order to prepare the polyol with all bio-based components as raw materials, cottonseed oil was first epoxidized by peroxyformic acid generated in situ from hydrogen peroxide and formic acid, and the cottonseed oil based polyols with variable hydroxyl value were then prepared by the ring-opening of epoxidized cottonseed oil with sorbitol, which is a multi-functional hydroxyl compound derived from a natural source. The chemical structure of the products was characterized with FTIR analysis, and the residual epoxy oxygen content and hydroxyl value of the polyol versus the ring-opening time were investigated.
In order to prepare the polyol with all bio-based components as raw materials, cottonseed oil was first epoxidized by peroxyformic acid generated in situ from hydrogen peroxide and formic acid, and the cottonseed oil based polyols with variable hydroxyl value were then prepared by the ring-opening of epoxidized cottonseed oil with sorbitol, which is a multi-functional hydroxyl compound derived from a natural source. The chemical structure of the products was characterized with FTIR analysis, and the residual epoxy oxygen content and hydroxyl value of the polyol versus the ring-opening time were investigated.
2011, 22(11): 1293-1296
doi: 10.1016/j.cclet.2011.06.014
Abstract:
A series of 3-ethoxy-4-hydroxybenzylidene/4-nitrobenzylidene hydrazides (1-20) was synthesized and tested for in vitro antimicrobial activity. The results of antimicrobial studies indicated that the compounds having dinitro, methoxy, hydroxy and nitro substituents on phenyl ring of the aromatic acids were most active ones. The QSAR investigation indicated the importance of the topological parameter, third order molecular connectivity index (3χ) in describing the antimicrobial activity of synthesized hydrazides.
A series of 3-ethoxy-4-hydroxybenzylidene/4-nitrobenzylidene hydrazides (1-20) was synthesized and tested for in vitro antimicrobial activity. The results of antimicrobial studies indicated that the compounds having dinitro, methoxy, hydroxy and nitro substituents on phenyl ring of the aromatic acids were most active ones. The QSAR investigation indicated the importance of the topological parameter, third order molecular connectivity index (3χ) in describing the antimicrobial activity of synthesized hydrazides.
2011, 22(11): 1297-1230
doi: 10.1016/j.cclet.2011.05.042
Abstract:
A novel 5-((4-(6, 7-dihydrothieno[3, 2-c]pyridin-5(4H)-ylsulfonyl)phenylamino)methyl)quinolin-8-ol (HTPSMQol) was synthesized by optimized reaction of 4-(6, 7-dihydrothieno[3, 2-c]pyridin-5(4H)-ylsulfonyl)aniline with 5-chloromethyI-8-hydroxy_quinoline hydrochloride (CMHQ). Also complexes of HTPSMQol were prepared by using various M (Ⅱ) metal salts. All compounds were analyzed by spectroscopic techniques and screened against various strains of microorganisms. The results showed higher antimicrobial activity of HTPSMQol compared to its metal complexes and comparable with Ciprofloxacin.
A novel 5-((4-(6, 7-dihydrothieno[3, 2-c]pyridin-5(4H)-ylsulfonyl)phenylamino)methyl)quinolin-8-ol (HTPSMQol) was synthesized by optimized reaction of 4-(6, 7-dihydrothieno[3, 2-c]pyridin-5(4H)-ylsulfonyl)aniline with 5-chloromethyI-8-hydroxy_quinoline hydrochloride (CMHQ). Also complexes of HTPSMQol were prepared by using various M (Ⅱ) metal salts. All compounds were analyzed by spectroscopic techniques and screened against various strains of microorganisms. The results showed higher antimicrobial activity of HTPSMQol compared to its metal complexes and comparable with Ciprofloxacin.
2011, 22(11): 1301-1304
doi: 10.1016/j.cclet.2011.05.039
Abstract:
A novel squaraine dye (SQ) modified by ferrocene has been synthesized through (E)-l-dodecyl-2-ferrocenyl vinyl-1H-pyrrole and squaric acid. The molecular structure of SQ was characterized by 1H NMR, 13C NMR, MS and elemental analysis. SQ is high soluble in common solvents. The maximum absorptions of SQ in different solvents are in the range of 708-734 nm, exhibiting positive solvatochromism with increasing solvent polarity. The optical and electrical properties of SQ indicate that it is a promising electron donor material for bulk-heterojunction organic solar cell.
A novel squaraine dye (SQ) modified by ferrocene has been synthesized through (E)-l-dodecyl-2-ferrocenyl vinyl-1H-pyrrole and squaric acid. The molecular structure of SQ was characterized by 1H NMR, 13C NMR, MS and elemental analysis. SQ is high soluble in common solvents. The maximum absorptions of SQ in different solvents are in the range of 708-734 nm, exhibiting positive solvatochromism with increasing solvent polarity. The optical and electrical properties of SQ indicate that it is a promising electron donor material for bulk-heterojunction organic solar cell.
2011, 22(11): 1305-1308
doi: 10.1016/j.cclet.2011.07.004
Abstract:
An environmentally friendly synthesis method for bis(indolyl)methanes has been developed in the presence of sodium lauryl ether sulfate (SLES), electrophilic substitution reactions of indoles with aldehydes were accomplished in water as solvent at room temperature without any Bronested or Lewis acid catalysts.
An environmentally friendly synthesis method for bis(indolyl)methanes has been developed in the presence of sodium lauryl ether sulfate (SLES), electrophilic substitution reactions of indoles with aldehydes were accomplished in water as solvent at room temperature without any Bronested or Lewis acid catalysts.
2011, 22(11): 1309-1312
doi: 10.1016/j.cclet.2011.06.012
Abstract:
The synthesis and labeling of 99mTc-N3-{N'-[2-sulfanyl-ethylamino)acetyl]-2-aminoethyl-sulfanyl-l-hexanamide}thymidine (99mTc-NHT) were studied. In the presence of sodium glucoheptonate (GH) and ethylene diamine tetraacetic acid (EDTA), 99mTc-NHT was obtained by using bisaminoethanethiol (N2S2) as a bifunctional coupling agent. The radiochemical purity of the 99mTc-NHT was over 95%. Biodistribution of 99mTc-NHT was performed in hepatoma HepA tumor-bearing mice. At 2 h p. i., the ratios of tumor-to-muscle, tumor-to-bone and tumor-to-blood were 4.41±0.32, 2.45±0.24 and 1.51±0.18, respectively.
The synthesis and labeling of 99mTc-N3-{N'-[2-sulfanyl-ethylamino)acetyl]-2-aminoethyl-sulfanyl-l-hexanamide}thymidine (99mTc-NHT) were studied. In the presence of sodium glucoheptonate (GH) and ethylene diamine tetraacetic acid (EDTA), 99mTc-NHT was obtained by using bisaminoethanethiol (N2S2) as a bifunctional coupling agent. The radiochemical purity of the 99mTc-NHT was over 95%. Biodistribution of 99mTc-NHT was performed in hepatoma HepA tumor-bearing mice. At 2 h p. i., the ratios of tumor-to-muscle, tumor-to-bone and tumor-to-blood were 4.41±0.32, 2.45±0.24 and 1.51±0.18, respectively.
2011, 22(11): 1313-1316
doi: 10.1016/j.cclet.2011.06.009
Abstract:
Melamine-formaldehyde resin supported H+ is used as an efficient catalyst in the Pechmann condensation reaction of phenols with β-ketoesters, in solvent-free media leading to the formation of coumarin derivatives using conventional heating and microwave irradiation in excellent yields with good purity.
Melamine-formaldehyde resin supported H+ is used as an efficient catalyst in the Pechmann condensation reaction of phenols with β-ketoesters, in solvent-free media leading to the formation of coumarin derivatives using conventional heating and microwave irradiation in excellent yields with good purity.
2011, 22(11): 1317-1320
doi: 10.1016/j.cclet.2011.06.008
Abstract:
A series of 2, 3-dihydroquinazolin-4(1H)-ones have been synthesized in good to excellent yields through direct cyclocondensa-tion of anthranilamide and aryl aldehydes or ketones in water or methanol under mild conditions. The reaction was efficiently promoted by 10 mol% sulfamic acid (SA, H2NSO3H) and the catalyst could be recovered easily after the reactions and reused without evident loss of reactivity.
A series of 2, 3-dihydroquinazolin-4(1H)-ones have been synthesized in good to excellent yields through direct cyclocondensa-tion of anthranilamide and aryl aldehydes or ketones in water or methanol under mild conditions. The reaction was efficiently promoted by 10 mol% sulfamic acid (SA, H2NSO3H) and the catalyst could be recovered easily after the reactions and reused without evident loss of reactivity.
2011, 22(11): 1321-1325
doi: 10.1016/j.cclet.2011.06.015
Abstract:
A series of MoTe0.15V0.1PxOn catalysts supported on the SiC were prepared by incipient wetness impregnation. The addition of P to MoTe0.15V0.1On/SiC catalysts improved the catalytic performance of selective oxidation from propane to acrolein (ACR), and the catalyst showed highest selectivity (33.7%) and yield (10.7%) when x=0.05. The MoTe0.15V0.1PxOn/SiC catalysts have been characterized by XRD, H2-TPR, Raman, XPS and NH3-TPD. The results indicated that a little H3PMo12O40 heteropoly acid and (VO)2P2O7 formed and MoO3 phase lessened after addition of P. The addition of P promoted the active species dispersed, increased the acidity on the surface, as well as might make the redox process easier. These significant differences improved the activity and selectivity of ACR.
A series of MoTe0.15V0.1PxOn catalysts supported on the SiC were prepared by incipient wetness impregnation. The addition of P to MoTe0.15V0.1On/SiC catalysts improved the catalytic performance of selective oxidation from propane to acrolein (ACR), and the catalyst showed highest selectivity (33.7%) and yield (10.7%) when x=0.05. The MoTe0.15V0.1PxOn/SiC catalysts have been characterized by XRD, H2-TPR, Raman, XPS and NH3-TPD. The results indicated that a little H3PMo12O40 heteropoly acid and (VO)2P2O7 formed and MoO3 phase lessened after addition of P. The addition of P promoted the active species dispersed, increased the acidity on the surface, as well as might make the redox process easier. These significant differences improved the activity and selectivity of ACR.
2011, 22(11): 1326-1330
doi: 10.1016/j.cclet.2011.05.025
Abstract:
Three novel conjugated polymers bearing 3, 4-bis(4-hexylthiophen-2-yl)-3-cyclobutene-l, 2-dione unit in their main chain have been synthesized successfully in good yields through Suzuki or Stille coupling reaction. Their molecular structures have been confirmed by FT-IR, 1H NMR and 13C NMR. All these copolymers exhibit broad and strong absorption bands in UV-vis region, and their optical band gaps are calculated to be 1.6-2.0 eV, suggesting that they have good coverage with the solar spectrum. These polymers have good thermostability and solubility in common organic solvents. Moreover, all these objective macromolecules possess high electron affinity of~3.8 eV determined from cyclic voltammetry measurement, implying that they are potential n-type polymeric photovoltaic materials.
Three novel conjugated polymers bearing 3, 4-bis(4-hexylthiophen-2-yl)-3-cyclobutene-l, 2-dione unit in their main chain have been synthesized successfully in good yields through Suzuki or Stille coupling reaction. Their molecular structures have been confirmed by FT-IR, 1H NMR and 13C NMR. All these copolymers exhibit broad and strong absorption bands in UV-vis region, and their optical band gaps are calculated to be 1.6-2.0 eV, suggesting that they have good coverage with the solar spectrum. These polymers have good thermostability and solubility in common organic solvents. Moreover, all these objective macromolecules possess high electron affinity of~3.8 eV determined from cyclic voltammetry measurement, implying that they are potential n-type polymeric photovoltaic materials.
2011, 22(11): 1331-1334
doi: 10.1016/j.cclet.2011.07.014
Abstract:
From the aqueous extract of Acacia catechu, two new phenolic compounds (3R, 4R)-3-(3, 4-dihydroxyphenyl)-4-hydroxycy-clohexanone (1) and (4R)-5-(l-(3, 4-dihydrophenyl)-3-oxoburyl)-dihydrofuran-2(3H)-one (2) were obtained. Their structures were determined on the basis of spectroscopic analysis. Free-radical scavenging activities of them were evaluated.
From the aqueous extract of Acacia catechu, two new phenolic compounds (3R, 4R)-3-(3, 4-dihydroxyphenyl)-4-hydroxycy-clohexanone (1) and (4R)-5-(l-(3, 4-dihydrophenyl)-3-oxoburyl)-dihydrofuran-2(3H)-one (2) were obtained. Their structures were determined on the basis of spectroscopic analysis. Free-radical scavenging activities of them were evaluated.
2011, 22(11): 1335-1338
doi: 10.1016/j.cclet.2011.07.001
Abstract:
The NIR micro-images of ibuprofen tablets were collected in this research. Compare correlation imaging and principal component analysis (PCA) with histogram were applied to acquire the spatial distribution of ibuprofen granule. The result indicated that a similar distribution trend can be acquired by both of the two methods mentioned above; the information of PC2 results from ibuprofen mainly since the correlation coefficient between PC2 loading vector and the NIR spectrum of ibuprofen is 0.9930. The result of PCA indicated that the information of PC2 results from ibuprofen mainly for both the low and the high content of ibuprofen in the tablets. The correlation coefficient between the data of the two PC2 loading vectors of the low and the high content of ibuprofen in the tablets is 0.9998, which indicates that the result of PCA is stable and reliable.
The NIR micro-images of ibuprofen tablets were collected in this research. Compare correlation imaging and principal component analysis (PCA) with histogram were applied to acquire the spatial distribution of ibuprofen granule. The result indicated that a similar distribution trend can be acquired by both of the two methods mentioned above; the information of PC2 results from ibuprofen mainly since the correlation coefficient between PC2 loading vector and the NIR spectrum of ibuprofen is 0.9930. The result of PCA indicated that the information of PC2 results from ibuprofen mainly for both the low and the high content of ibuprofen in the tablets. The correlation coefficient between the data of the two PC2 loading vectors of the low and the high content of ibuprofen in the tablets is 0.9998, which indicates that the result of PCA is stable and reliable.
2011, 22(11): 1339-1342
doi: 10.1016/j.cclet.2011.05.038
Abstract:
Wedged and V-shaped cells have advantages on depressing strong absorption bands and keeping the photo windows wide open without absorption block. Alternatively, this work presents a concave cell design, which is constructed by a plano-convex CaF2 lens in combination with a flat plate. Mathematical equations have been provided for data treatment with Matlab programs. The result indicates that the concave cell has advantages similar to the V-shaped cell. Reflection-absorption measurements of ethanol have been conducted on the cell in mid-IR region for demonstration. The spectrum obtained from the concave cell can easily be interpreted to regenerate its normal spectrum, which is fitting well with the spectrum taken in a conventional thin-layer cell. The concave cell is easier to construct and more convenient to operate, willing to have popular usages.
Wedged and V-shaped cells have advantages on depressing strong absorption bands and keeping the photo windows wide open without absorption block. Alternatively, this work presents a concave cell design, which is constructed by a plano-convex CaF2 lens in combination with a flat plate. Mathematical equations have been provided for data treatment with Matlab programs. The result indicates that the concave cell has advantages similar to the V-shaped cell. Reflection-absorption measurements of ethanol have been conducted on the cell in mid-IR region for demonstration. The spectrum obtained from the concave cell can easily be interpreted to regenerate its normal spectrum, which is fitting well with the spectrum taken in a conventional thin-layer cell. The concave cell is easier to construct and more convenient to operate, willing to have popular usages.
2011, 22(11): 1343-1346
doi: 10.1016/j.cclet.2011.05.028
Abstract:
Apolipoprotein B100 (apoB-100) is a major protein of the cholesterol-rich low-density lipoprotein (LDL) and reflects a better assessment of total atherogenic burden to the vascular system than LDL. In this work, a simple and sensitive method has been developed to determine picoliter apoB-100s using the PMMA microfluidic chip coupled with electrochemical detection system. This method performs very well with a detectable linear range of 1-800 pg/mL and a detection limit of 1 pg/mL. A real serum sample has further been detected by this microchip-based biosensor. The results show that this kind of method is practicable and has the potential application in clinical analysis and diagnosis.
Apolipoprotein B100 (apoB-100) is a major protein of the cholesterol-rich low-density lipoprotein (LDL) and reflects a better assessment of total atherogenic burden to the vascular system than LDL. In this work, a simple and sensitive method has been developed to determine picoliter apoB-100s using the PMMA microfluidic chip coupled with electrochemical detection system. This method performs very well with a detectable linear range of 1-800 pg/mL and a detection limit of 1 pg/mL. A real serum sample has further been detected by this microchip-based biosensor. The results show that this kind of method is practicable and has the potential application in clinical analysis and diagnosis.
2011, 22(11): 1347-1350
doi: 10.1016/j.cclet.2011.05.029
Abstract:
This study reveals that the noncovalent complexation between β-CD and Cu(HMTA)2+ makes a positive contribution to the coordination interaction between Cu2+ and HMTA in a tricomponent system. Besides, mono-and binuclear complexes:[β-CD·Cu]+ and[Cu-β-CD·Cu)+ were observed under the condition of ESI-MS.
This study reveals that the noncovalent complexation between β-CD and Cu(HMTA)2+ makes a positive contribution to the coordination interaction between Cu2+ and HMTA in a tricomponent system. Besides, mono-and binuclear complexes:[β-CD·Cu]+ and[Cu-β-CD·Cu)+ were observed under the condition of ESI-MS.
2011, 22(11): 1351-1354
doi: 10.1016/j.cclet.2011.05.044
Abstract:
Synthetic materials that can specifically recognize proteins will find wide application in many fields. In this report, bovine serum albumin was chosen as the template protein. Acrylamide and N, N'-methylenebisacrylamide were employed as the functional and cross-linker monomers, respectively. Molecularly imprinted macroporous monolithic materials that can preferentially bind the template protein in an aqueous environment were prepared by combination of molecular imprinting technique and freezing/thawing preparation method. The resulted imprinted macroporous monolithic columns were evaluated by utilizing as stationary phase in high performance liquid chromatography and solid-phase extraction materials. The experimental results indicated that the imprinted macroporous monolithic column exhibited good recognition for template protein, as compared with the control protein (hemoglobin), whereas the non-imprinted polymer (prepared under the same conditions except without addition template protein) had no selective properties.
Synthetic materials that can specifically recognize proteins will find wide application in many fields. In this report, bovine serum albumin was chosen as the template protein. Acrylamide and N, N'-methylenebisacrylamide were employed as the functional and cross-linker monomers, respectively. Molecularly imprinted macroporous monolithic materials that can preferentially bind the template protein in an aqueous environment were prepared by combination of molecular imprinting technique and freezing/thawing preparation method. The resulted imprinted macroporous monolithic columns were evaluated by utilizing as stationary phase in high performance liquid chromatography and solid-phase extraction materials. The experimental results indicated that the imprinted macroporous monolithic column exhibited good recognition for template protein, as compared with the control protein (hemoglobin), whereas the non-imprinted polymer (prepared under the same conditions except without addition template protein) had no selective properties.
2011, 22(11): 1355-1358
doi: 10.1016/j.cclet.2011.06.013
Abstract:
5-[(4'-Heptoxy-4-biphenylyl)carbonyloxy]-l-pentyne (A-3, 7) was synthesized and the phase structures and transitions were investigated by differential scanning calorimetry (DSC), wide angle X-ray diffraction (WAXD), polarized light microscopy (PLM) and the molecular packing in the crystal and liquid crystalline phases were simulated by molecular dynamic simulation. The results showed that the sample formed thermodynamically metastable SmA and SmC2 phases before crystallized during cooling and the crystal phase directly transformed into isotropic phase during heating.
5-[(4'-Heptoxy-4-biphenylyl)carbonyloxy]-l-pentyne (A-3, 7) was synthesized and the phase structures and transitions were investigated by differential scanning calorimetry (DSC), wide angle X-ray diffraction (WAXD), polarized light microscopy (PLM) and the molecular packing in the crystal and liquid crystalline phases were simulated by molecular dynamic simulation. The results showed that the sample formed thermodynamically metastable SmA and SmC2 phases before crystallized during cooling and the crystal phase directly transformed into isotropic phase during heating.
2011, 22(11): 1359-1362
doi: 10.1016/j.cclet.2011.07.003
Abstract:
TeOx-SiO2 composite films having third-order nonlinearities were prepared by electrochemically induced sol-gel deposition method on ITO substrate. The third-order optical nonlinearities of the films were measured by Z-scan technique. The third-order nonlinear susceptibilities (χ(3)) of the as-prepared films are 5.9×10-7 to 4.29×10-6 esu. The surface morphology and composition of the films were characterized by SEM/EDX, which identified that Te metallic particles well dispersed in TeOx-SiO2 gel films.
TeOx-SiO2 composite films having third-order nonlinearities were prepared by electrochemically induced sol-gel deposition method on ITO substrate. The third-order optical nonlinearities of the films were measured by Z-scan technique. The third-order nonlinear susceptibilities (χ(3)) of the as-prepared films are 5.9×10-7 to 4.29×10-6 esu. The surface morphology and composition of the films were characterized by SEM/EDX, which identified that Te metallic particles well dispersed in TeOx-SiO2 gel films.
2011, 22(11): 1363-1366
doi: 10.1016/j.cclet.2011.05.041
Abstract:
Biodiesel was synthesized from soybean oil by transesterification over Li2SiO3 catalyst. The Li2SiO3 can be used for biodiesel production directly without further drying or thermal pretreatment, no obvious difference in the FAME conversion (92.4-96.7%) between the air-exposed catalyst (24-72 h) and the fresh one (94.2%). This leads to important benefits when considering industrial applications of Li2SiO3 as a solid catalyst for storing and handling catalyst without taking special actions.
Biodiesel was synthesized from soybean oil by transesterification over Li2SiO3 catalyst. The Li2SiO3 can be used for biodiesel production directly without further drying or thermal pretreatment, no obvious difference in the FAME conversion (92.4-96.7%) between the air-exposed catalyst (24-72 h) and the fresh one (94.2%). This leads to important benefits when considering industrial applications of Li2SiO3 as a solid catalyst for storing and handling catalyst without taking special actions.
2011, 22(11): 1367-1370
doi: 10.1016/j.cclet.2011.05.006
Abstract:
A series of new fluoro-containing copolymers have been synthesized by a Mitsunobu reaction with 4, 4'-(hexafluoro-isopropylidene)bisphenol A (6FBPA) and the corresponding N, N-dihydroxyethylaminoaryl azo or ring-locked triene compounds, which have high thermal stability and good solubility in organic solvents. The nonlinear optical (NLO) measurements made by Marker fringe method at 1064 nm indicate that the copolymers embedded with the ring-locked triene and azo chromophores exhibit higher macroscopic nonlinear optical coefficient (70.2 pm/V and 26.5-34.6 pm/V, respectively). Thermal analysis and UV-visible absorption spectra show that the copolymers have good thermal stability (Td=264-319℃) and optical transparency (λmax<500nm).
A series of new fluoro-containing copolymers have been synthesized by a Mitsunobu reaction with 4, 4'-(hexafluoro-isopropylidene)bisphenol A (6FBPA) and the corresponding N, N-dihydroxyethylaminoaryl azo or ring-locked triene compounds, which have high thermal stability and good solubility in organic solvents. The nonlinear optical (NLO) measurements made by Marker fringe method at 1064 nm indicate that the copolymers embedded with the ring-locked triene and azo chromophores exhibit higher macroscopic nonlinear optical coefficient (70.2 pm/V and 26.5-34.6 pm/V, respectively). Thermal analysis and UV-visible absorption spectra show that the copolymers have good thermal stability (Td=264-319℃) and optical transparency (λmax<500nm).
2011, 22(11): 1371-1374
doi: 10.1016/j.cclet.2011.05.004
Abstract:
The novel functionalized triblock copolymers, poly[(4-vinylphenyl)dimethylsilane]-b-polybutadiene-b-poly[(4-vinylphenyl)-dimethylsilane] (PVPDMS-b-PBd-b-PVPDMS), were synthesized by anionic polymerization method using high vacuum technique. The hydrocarbon-soluble dilithium initiator synthesized from 1, 3-di[l-(methylphenyl)ethenyl]benzene (MPEB) was used to synthesize polybutadiene (PBd) precursors and the triblock copolymers in the presence of sec-BuOLi. The precursors and copolymers were characterized by size exclusion chromatography (SEC), 1HNMR and DSC techniques.
The novel functionalized triblock copolymers, poly[(4-vinylphenyl)dimethylsilane]-b-polybutadiene-b-poly[(4-vinylphenyl)-dimethylsilane] (PVPDMS-b-PBd-b-PVPDMS), were synthesized by anionic polymerization method using high vacuum technique. The hydrocarbon-soluble dilithium initiator synthesized from 1, 3-di[l-(methylphenyl)ethenyl]benzene (MPEB) was used to synthesize polybutadiene (PBd) precursors and the triblock copolymers in the presence of sec-BuOLi. The precursors and copolymers were characterized by size exclusion chromatography (SEC), 1HNMR and DSC techniques.
2011, 22(11): 1375-1378
doi: 10.1016/j.cclet.2011.05.024
Abstract:
Three polymer-amphiphile complexes were prepared by combining poly(allylamine hydrochloride) (PAH) with the potassium salt of mono-, di-, and trisubstituted benzoic acid dendrons (4-octyloxybenzoic acid, 3, 5-dioctyloxybenzoic acid, and 3, 4, 5-trioctyloxybenzoic acid). The solid structure and properties were monitored with FT-IR, XRD, TG, DSC, and polarized optical microscope (POM). Difference in the tail chain number of the dendritic amphiphile induced two different mesomorphous structures:lamella for the mono-, disubstituted dendron containing complexes and hexagonal column for the trisubstituted dendron containing complexes. These corresponded to the ionic thermotropic liquid crystal SmA and φh phases, respectively. This finding is significant for design of functional nanostructures based on the ionic complexation of polymers and amphiphiles.
Three polymer-amphiphile complexes were prepared by combining poly(allylamine hydrochloride) (PAH) with the potassium salt of mono-, di-, and trisubstituted benzoic acid dendrons (4-octyloxybenzoic acid, 3, 5-dioctyloxybenzoic acid, and 3, 4, 5-trioctyloxybenzoic acid). The solid structure and properties were monitored with FT-IR, XRD, TG, DSC, and polarized optical microscope (POM). Difference in the tail chain number of the dendritic amphiphile induced two different mesomorphous structures:lamella for the mono-, disubstituted dendron containing complexes and hexagonal column for the trisubstituted dendron containing complexes. These corresponded to the ionic thermotropic liquid crystal SmA and φh phases, respectively. This finding is significant for design of functional nanostructures based on the ionic complexation of polymers and amphiphiles.
2011, 22(11): 1379-1382
doi: 10.1016/j.cclet.2011.05.037
Abstract:
In this study, we compared the effect of n-pentane and ice-water bath on removing the thermal effect in the poly (p-phenylene terephthalamide) (PPTA) polymerization process. The results indicate that the n-pentane can help to transfer the reaction heat faster and better. Adding suitable amount of n-pentanes into the PPTA preparation process not only improve the heat transfer, but also reduce the motor power in the polymerization process. Moreover, the introduction of n-pentane properly does not result in decrease of the inherent viscosity (ηinh) of polymer. Instead, it leads to increased viscosity of polymer during the PPTA preparation process. The results indicate that n-pentane can effectively transfer the reaction heat and avoid overheating during the polymerization of PPTA.
In this study, we compared the effect of n-pentane and ice-water bath on removing the thermal effect in the poly (p-phenylene terephthalamide) (PPTA) polymerization process. The results indicate that the n-pentane can help to transfer the reaction heat faster and better. Adding suitable amount of n-pentanes into the PPTA preparation process not only improve the heat transfer, but also reduce the motor power in the polymerization process. Moreover, the introduction of n-pentane properly does not result in decrease of the inherent viscosity (ηinh) of polymer. Instead, it leads to increased viscosity of polymer during the PPTA preparation process. The results indicate that n-pentane can effectively transfer the reaction heat and avoid overheating during the polymerization of PPTA.
2011, 22(11): 1383-1386
doi: 10.1016/j.cclet.2011.04.017
Abstract:
Theoretical investigations have been performed to explore the variation in electronic, optical, and charge transport properties upon the change of the chemical composition along the backbone in 2, 1, 3-benzothiadiazole (BTD)-based derivative. Narrow difference between hole and electron transportations with the charge hopping model indicates studied BTD-based derivative can be used as good ambipolar transport material in organic light-emitting diodes.
Theoretical investigations have been performed to explore the variation in electronic, optical, and charge transport properties upon the change of the chemical composition along the backbone in 2, 1, 3-benzothiadiazole (BTD)-based derivative. Narrow difference between hole and electron transportations with the charge hopping model indicates studied BTD-based derivative can be used as good ambipolar transport material in organic light-emitting diodes.
