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2002 Volume 13 Issue 9
2002, 13(9): 809-810
Abstract:
Reduction of δ-alkoxy enal 1 and 4 by sodium borohydride in methanol with a catalytic amount of magnesium methoxide gave unexpected methoxylated poducts 3 and 6 respectively.
Reduction of δ-alkoxy enal 1 and 4 by sodium borohydride in methanol with a catalytic amount of magnesium methoxide gave unexpected methoxylated poducts 3 and 6 respectively.
2002, 13(9): 811-813
Abstract:
From natural tartaric acid, (R)-2-benzyloxy-3-(2-tetrahydropyranyloxy) propanol 3 was designed and synthesized, and (R)-2-benzyloxy-3-(4-methoxybenzyloxy) propanol 7 was prepared in a new method. They can be used as chiral synthons of lysophosphatidic acid and other compounds with asymmetric propanetriol backbone.
From natural tartaric acid, (R)-2-benzyloxy-3-(2-tetrahydropyranyloxy) propanol 3 was designed and synthesized, and (R)-2-benzyloxy-3-(4-methoxybenzyloxy) propanol 7 was prepared in a new method. They can be used as chiral synthons of lysophosphatidic acid and other compounds with asymmetric propanetriol backbone.
Synthesis and Their Endothelium Vascular Relaxation of Arecoline Derivatives Containing Oxadiazoline
2002, 13(9): 814-817
Abstract:
Ten novel 1,1-dimethyl-3-(2-or 5-aryl-4-acetyl-2,3-dihydro-1,3,4-oxadiazoline-5-or-2-yl)-1,2,5,6-tetrahydropyridinium iodides were synthesized from starting material nicotinalde-hyde or nicotinic acid by two different synthetic methods respectively. The preliminary bioactive tests indicate som compounds exhibit potent relaxing effect on endothelial cells, comparable to Ach or arecoline.
Ten novel 1,1-dimethyl-3-(2-or 5-aryl-4-acetyl-2,3-dihydro-1,3,4-oxadiazoline-5-or-2-yl)-1,2,5,6-tetrahydropyridinium iodides were synthesized from starting material nicotinalde-hyde or nicotinic acid by two different synthetic methods respectively. The preliminary bioactive tests indicate som compounds exhibit potent relaxing effect on endothelial cells, comparable to Ach or arecoline.
2002, 13(9): 818-819
Abstract:
Reaction of simple dialkyl phosphites with symmetrical 1,3,5-trisubstituted hexahydro-triazines (HHTs) in the presence of benzyl chloride, afforded tertiaryaminomethylphosphonates in excellent yields. Glyphosate, α-aminomethylphosphonates and their derivatives can therefore be synthesized by this procedure conveniently.
Reaction of simple dialkyl phosphites with symmetrical 1,3,5-trisubstituted hexahydro-triazines (HHTs) in the presence of benzyl chloride, afforded tertiaryaminomethylphosphonates in excellent yields. Glyphosate, α-aminomethylphosphonates and their derivatives can therefore be synthesized by this procedure conveniently.
2002, 13(9): 820-823
Abstract:
The synthesis of epoxy aldehyde 4, a cyclization precursor for the total synthesis of 14-deoxycrassin and pseudoplexaurol, starting from geraniol in a convergent and stereoselective manner, is described.
The synthesis of epoxy aldehyde 4, a cyclization precursor for the total synthesis of 14-deoxycrassin and pseudoplexaurol, starting from geraniol in a convergent and stereoselective manner, is described.
2002, 13(9): 824-825
Abstract:
A series of novel aromatic poly (amide imide)s containing phthalazinone moieties were prepared from 2-(4-aminophenyl)-4-[3-methyl-4-(4-aminophenoxy)-2,3-phthalazinone-1], a novel diamine 1 with four diimide-dicarboxylic acids by Yamazaki phosphorylation method with the inherent viscosity of 0.36~0.65 dL/g. These polymers had high glass transition temperatures above 300℃ and they lost 10% weight between 426~475℃ in N2. The structure of diamine 1 and the polymers was confirmed by IR, 1H NMR and MS. The obtained polymers were readily soluble in polar solvents such as NMP, m-cresol etc. and easily cast into tough, flexible films. The X-ray indicated that they are all amorphous.
A series of novel aromatic poly (amide imide)s containing phthalazinone moieties were prepared from 2-(4-aminophenyl)-4-[3-methyl-4-(4-aminophenoxy)-2,3-phthalazinone-1], a novel diamine 1 with four diimide-dicarboxylic acids by Yamazaki phosphorylation method with the inherent viscosity of 0.36~0.65 dL/g. These polymers had high glass transition temperatures above 300℃ and they lost 10% weight between 426~475℃ in N2. The structure of diamine 1 and the polymers was confirmed by IR, 1H NMR and MS. The obtained polymers were readily soluble in polar solvents such as NMP, m-cresol etc. and easily cast into tough, flexible films. The X-ray indicated that they are all amorphous.
2002, 13(9): 826-829
Abstract:
Dialkyl 2-phenylfuran (and 2-phenyltetrahydrofuran)-3,4-dicarboxylates (1, 2, 5-7), which are potential precursors of the synthesis of furofuran and tetrahydrofurofuran lignans, can be selectively hydrolyzed to monoacid (3, 8) by potassium hydroxide. The regioselective hydrolysis was affected significantly by the 2-phenyl group of the furan or tetrahydrofuran skeleton. The geometric structures of 3, 8 and related compounds were elucidated and verified by NMR spectra.
Dialkyl 2-phenylfuran (and 2-phenyltetrahydrofuran)-3,4-dicarboxylates (1, 2, 5-7), which are potential precursors of the synthesis of furofuran and tetrahydrofurofuran lignans, can be selectively hydrolyzed to monoacid (3, 8) by potassium hydroxide. The regioselective hydrolysis was affected significantly by the 2-phenyl group of the furan or tetrahydrofuran skeleton. The geometric structures of 3, 8 and related compounds were elucidated and verified by NMR spectra.
2002, 13(9): 830-831
Abstract:
The first total synthesis of (±)-Celaphanol A was accomplished starting from α-cyclocitral and 3,4-dimethoxy benzyl chloride via a six-step process, in which the intramolecular cyclization of ketone 4 with BF3·Et2O afforded an all-cis isomer intermediate for synthesis of aromatic tricyclic diterpenes.
The first total synthesis of (±)-Celaphanol A was accomplished starting from α-cyclocitral and 3,4-dimethoxy benzyl chloride via a six-step process, in which the intramolecular cyclization of ketone 4 with BF3·Et2O afforded an all-cis isomer intermediate for synthesis of aromatic tricyclic diterpenes.
2002, 13(9): 832-835
Abstract:
2-O-Acetonyl-β-cyclodextrin with a suitable average substitution degree of about 5.8,which could be used as a key intermediate for water soluble functional β-cyclodextrin derivatives,was prepared based on the proper oxidation of heptakis (6-O-dimethyl-tert-butylsilyl)-2-O-hydroxypropyl-β-cyclodextrin.
2-O-Acetonyl-β-cyclodextrin with a suitable average substitution degree of about 5.8,which could be used as a key intermediate for water soluble functional β-cyclodextrin derivatives,was prepared based on the proper oxidation of heptakis (6-O-dimethyl-tert-butylsilyl)-2-O-hydroxypropyl-β-cyclodextrin.
2002, 13(9): 836-838
Abstract:
The reaction of bis-benzimidazolium salts with sodium hydrogen telluride is reported,and a new synthetic method for dialdehydes is provided.
The reaction of bis-benzimidazolium salts with sodium hydrogen telluride is reported,and a new synthetic method for dialdehydes is provided.
2002, 13(9): 839-842
Abstract:
The highly water-soluble phosphine ligands Na2O3PCH2CH2NH(CH2CH2O)nCH2CH2N(CH2PPh2)2 (n=1,2,3) were prepared by a new and simple route under mild conditions in goodyield; the palladium (Ⅱ) complexes of the ligands 3a~c with 2:1 or 4:1-PPh2 to Pd2+ molar ratiowere also prepared and characterized.
The highly water-soluble phosphine ligands Na2O3PCH2CH2NH(CH2CH2O)nCH2CH2N(CH2PPh2)2 (n=1,2,3) were prepared by a new and simple route under mild conditions in goodyield; the palladium (Ⅱ) complexes of the ligands 3a~c with 2:1 or 4:1-PPh2 to Pd2+ molar ratiowere also prepared and characterized.
2002, 13(9): 843-844
Abstract:
Bis(8-quinolinolato)zirconium dichloride (Ox)2ZrCl2 (Ox-=8-quinolinolato) was foundactive for ethylene oligomerization with a high selectivity of 84~94% to C4~C10 olefins at70~100℃ under the pressure of 1.8 MPa using Et2AlCl as a co-catalyst (Al/Zr=60).
Bis(8-quinolinolato)zirconium dichloride (Ox)2ZrCl2 (Ox-=8-quinolinolato) was foundactive for ethylene oligomerization with a high selectivity of 84~94% to C4~C10 olefins at70~100℃ under the pressure of 1.8 MPa using Et2AlCl as a co-catalyst (Al/Zr=60).
2002, 13(9): 845-848
Abstract:
A polyclonal antibody against the currently concerned estrogenic bisphcnol compoundswas produced according to a new scheme. 4,4-Bis (4-hydroxyphenyl) valeric acid was used tosynthesize the complete antigen in which the characteristic bisphenol structure was exposed to thelargest extent. The produced polyclonal antibody showed high specificity and affinity forbisphenol A.
A polyclonal antibody against the currently concerned estrogenic bisphcnol compoundswas produced according to a new scheme. 4,4-Bis (4-hydroxyphenyl) valeric acid was used tosynthesize the complete antigen in which the characteristic bisphenol structure was exposed to thelargest extent. The produced polyclonal antibody showed high specificity and affinity forbisphenol A.
2002, 13(9): 849-850
Abstract:
A new binary carbazole alkaloid, 8,8"-biskoenigine (1), along with its monomer,kocnigine, was isolated from the dried leaves of Murraya koenigii collected in Xishuangbanna,Yunnan province. The structure of 1 was established by spectroscopic methods.
A new binary carbazole alkaloid, 8,8"-biskoenigine (1), along with its monomer,kocnigine, was isolated from the dried leaves of Murraya koenigii collected in Xishuangbanna,Yunnan province. The structure of 1 was established by spectroscopic methods.
2002, 13(9): 851-854
Abstract:
Bioactivity-guided fractionation led to the isolation of a new steroidal saponin,orbiculatoside B, together with a pair of furostanol saponins, protobioside and methyl protobioside,from the fresh rhizomes of Dioscorea deltoidea Wall var. orbiculata. The new compound was identified to be isonarthogenin 3-O-α-L-rhamnopyranosyl (1→2)-[α-L-rhamnopyranosyl-(1→4)]-β-D-glucopyranoside by various NMR techniques in combination with chemical methods. The three saponins showed strong activity against Pyricularia oryzae, and were cytotoxic to cancer cell line K562, HCT-15, A549, and A2780a in vitro.
Bioactivity-guided fractionation led to the isolation of a new steroidal saponin,orbiculatoside B, together with a pair of furostanol saponins, protobioside and methyl protobioside,from the fresh rhizomes of Dioscorea deltoidea Wall var. orbiculata. The new compound was identified to be isonarthogenin 3-O-α-L-rhamnopyranosyl (1→2)-[α-L-rhamnopyranosyl-(1→4)]-β-D-glucopyranoside by various NMR techniques in combination with chemical methods. The three saponins showed strong activity against Pyricularia oryzae, and were cytotoxic to cancer cell line K562, HCT-15, A549, and A2780a in vitro.
2002, 13(9): 855-856
Abstract:
A new eudesmanoilde was isolated from the aerial parts of Carpesium macrocephalum.Its structure was elucidated as 2α-acetoxy-11αH-eudesma-4-en-12,8β-olide by spectral methods.
A new eudesmanoilde was isolated from the aerial parts of Carpesium macrocephalum.Its structure was elucidated as 2α-acetoxy-11αH-eudesma-4-en-12,8β-olide by spectral methods.
2002, 13(9): 857-858
Abstract:
A new dihydroflavone (1), named macrophyllol A, was isolated from the roots of Uvaria nacrophylla. Its structure was elucidated on the basis of spectroscopic evidence.
A new dihydroflavone (1), named macrophyllol A, was isolated from the roots of Uvaria nacrophylla. Its structure was elucidated on the basis of spectroscopic evidence.
2002, 13(9): 859-861
Abstract:
From the ethanolie Extract of the whole plant of Hemistepta lyrata Bunge.,a new lignan, named hemislin B Glucoside,has been isolated as α-(trans-3-methoxy-4-O-β-D-glucopyranosylbenzylidene)-β-(3,4-dimethoxybenzyl)-γ-butyrolactone. Its structure has been established on the basis of UV, IR, FABMS,1H-NMR,13C-NMR, HMQC and HMBC speetral analysis.
From the ethanolie Extract of the whole plant of Hemistepta lyrata Bunge.,a new lignan, named hemislin B Glucoside,has been isolated as α-(trans-3-methoxy-4-O-β-D-glucopyranosylbenzylidene)-β-(3,4-dimethoxybenzyl)-γ-butyrolactone. Its structure has been established on the basis of UV, IR, FABMS,1H-NMR,13C-NMR, HMQC and HMBC speetral analysis.
2002, 13(9): 862-864
Abstract:
1,2-methylenedioxy-9-methoxy-N-methoxycarbonyl-aporphine and 1,2-methylenedioxy-8,9-dimethoxy-N-methoxycarbonyl-aporphine, two new alkaloids possessing a N-(methoxy carbonyl) group have been isolated from the stems of Fssistigma bracteolatum. Their structures were established on the basis of spectral analysis.
1,2-methylenedioxy-9-methoxy-N-methoxycarbonyl-aporphine and 1,2-methylenedioxy-8,9-dimethoxy-N-methoxycarbonyl-aporphine, two new alkaloids possessing a N-(methoxy carbonyl) group have been isolated from the stems of Fssistigma bracteolatum. Their structures were established on the basis of spectral analysis.
2002, 13(9): 865-866
Abstract:
From the underground parts of Glehnia littoralis Fr. Schmidt ex Miquel (Umbelliferae), a new compound named glehnilate was obtained. Its structure was determined by analysis of its spectral data.
From the underground parts of Glehnia littoralis Fr. Schmidt ex Miquel (Umbelliferae), a new compound named glehnilate was obtained. Its structure was determined by analysis of its spectral data.
2002, 13(9): 867-870
Abstract:
An electrochemical method for detection of cortisol based on capillary electrophoretic enzyme immunoassay has been developed. A limit of detection of 1.7×10-9 mol/L was obtained.
An electrochemical method for detection of cortisol based on capillary electrophoretic enzyme immunoassay has been developed. A limit of detection of 1.7×10-9 mol/L was obtained.
2002, 13(9): 871-873
Abstract:
A Capillary electrophortic enzyme linked immunoassay with electrochemical detection (CE-EIA-ED) has been developed. The method can be used to determine thyroxine with a limit of 3.8×10-9 mol/L.
A Capillary electrophortic enzyme linked immunoassay with electrochemical detection (CE-EIA-ED) has been developed. The method can be used to determine thyroxine with a limit of 3.8×10-9 mol/L.
2002, 13(9): 874-876
Abstract:
A simple, rapid and low-cost method of separation and determination of homovanillic acid and vanillylmandelic acid in human urine was developed based on capillary zone electrophoresis/amperometric detection with high sensitivity and good resolution.
A simple, rapid and low-cost method of separation and determination of homovanillic acid and vanillylmandelic acid in human urine was developed based on capillary zone electrophoresis/amperometric detection with high sensitivity and good resolution.
2002, 13(9): 877-880
Abstract:
A microemulsion electrokinetic chromatography method has been firstly used for the separation of the therapeutically important xanthones from Securidaca inappendiculata. The separation of the nine xanthones was systematically optimized with respect to pH, composition of microemulsion, addition of cyclodextrins, applied voltage and column temperature. Baseline separation was successfully achieved for the nine xanthones, which was also compared with that by micellar electrokinetic chromatography
A microemulsion electrokinetic chromatography method has been firstly used for the separation of the therapeutically important xanthones from Securidaca inappendiculata. The separation of the nine xanthones was systematically optimized with respect to pH, composition of microemulsion, addition of cyclodextrins, applied voltage and column temperature. Baseline separation was successfully achieved for the nine xanthones, which was also compared with that by micellar electrokinetic chromatography
2002, 13(9): 881-882
Abstract:
Polyetherimide (PEI) was sulfonated by chlorosulfonic acid for the first time. The sulfonated products were characterized by FT-IR, DSC, ion exchange capacity and water sorption measurement. The hydrophilicity of PEI was improved by the sulfonation. The PEI was blended with the sodium salt form of sulfonated PEI (SPEI) to prepare microporous membranes. The morphologies of the membranes were studied with Scanning Electron Microscope (SEM).
Polyetherimide (PEI) was sulfonated by chlorosulfonic acid for the first time. The sulfonated products were characterized by FT-IR, DSC, ion exchange capacity and water sorption measurement. The hydrophilicity of PEI was improved by the sulfonation. The PEI was blended with the sodium salt form of sulfonated PEI (SPEI) to prepare microporous membranes. The morphologies of the membranes were studied with Scanning Electron Microscope (SEM).
2002, 13(9): 883-886
Abstract:
Fabrication of polyurethane molecular stamps (PU stamps) based on polypropylene glycol (PPG) and toluene diisocyanate (TDI), using 3,3'-dichloro-4,4'-methylenedianiline (MOCA) as the crosslinker, is reported. It was shown from the contact angle measurement that PU stamps surface has good affinity with acetonitrile, guaranteeing the well distribution of DNA monomers on patterned stamps. Laser confocal fluorescence microscopy images of oligonucleotide arrays after hybridization confirmed polyurethane is an excellent material for molecular stamps when transferring polar chemicals and conducting reactions on interfaces by stamping.
Fabrication of polyurethane molecular stamps (PU stamps) based on polypropylene glycol (PPG) and toluene diisocyanate (TDI), using 3,3'-dichloro-4,4'-methylenedianiline (MOCA) as the crosslinker, is reported. It was shown from the contact angle measurement that PU stamps surface has good affinity with acetonitrile, guaranteeing the well distribution of DNA monomers on patterned stamps. Laser confocal fluorescence microscopy images of oligonucleotide arrays after hybridization confirmed polyurethane is an excellent material for molecular stamps when transferring polar chemicals and conducting reactions on interfaces by stamping.
2002, 13(9): 887-890
Abstract:
Three rare-earth-containing heteropolyoxometalates with different sizes, Na9[Eu(W5O18)2], K13[Eu(SiW11O39)2], and K17[Eu(P2W17O61)2], have been incorporated by self-assembly into the interlayer of synthetic multibilayer films of dimethyldioctadecylammonium chloride and exhibited different orientations.
Three rare-earth-containing heteropolyoxometalates with different sizes, Na9[Eu(W5O18)2], K13[Eu(SiW11O39)2], and K17[Eu(P2W17O61)2], have been incorporated by self-assembly into the interlayer of synthetic multibilayer films of dimethyldioctadecylammonium chloride and exhibited different orientations.
2002, 13(9): 891-892
Abstract:
Nanoporous TiO2 photocatalysts were prepared by use of controlled drying method with surfactants. The surface area and porous properties are dependent on the chain length of incorporated surfactant cation. The TiO2 materials prepared in the presence of surfactant molecules during the gel formation exhibit much higher photocatalytic activity than that prepared in the absence of surfactants.
Nanoporous TiO2 photocatalysts were prepared by use of controlled drying method with surfactants. The surface area and porous properties are dependent on the chain length of incorporated surfactant cation. The TiO2 materials prepared in the presence of surfactant molecules during the gel formation exhibit much higher photocatalytic activity than that prepared in the absence of surfactants.
Nonlinear Optical Properties of Tri-nuclear Transition Metal Clusters M-μ-S)s-M'(M=Mo,W;M'=Cu,Ag,Au)
2002, 13(9): 893-896
Abstract:
The static polarizabilities and the second-order hyperpolarizabilities of a series of tri-nuclear metal cluster models MS4(M'PPh3)2(M'PPh3) (M=Mo,W;M'=Cu, Ag, Au) have been calculated within the first-principle theoretical framework. The model clusters have two fragments of rhombic units and it is the charge transfer from one of these moieties to the other that is responsible for nonlinear optical property. This kind of electronic delocalization, differentiated from that of planar π-system, is very interesting and is worthy for further investigation.
The static polarizabilities and the second-order hyperpolarizabilities of a series of tri-nuclear metal cluster models MS4(M'PPh3)2(M'PPh3) (M=Mo,W;M'=Cu, Ag, Au) have been calculated within the first-principle theoretical framework. The model clusters have two fragments of rhombic units and it is the charge transfer from one of these moieties to the other that is responsible for nonlinear optical property. This kind of electronic delocalization, differentiated from that of planar π-system, is very interesting and is worthy for further investigation.
2002, 13(9): 897-900
Abstract:
Biogenic isoprene emissions have been believed to be from only photosynthesis processes in plant. However nocturnal isoprene emission from pine is detected. And by feeding 13CO2 to plants, it is found that both photosynthesis pathway and light independent processes contribute to isoprene emissions.
Biogenic isoprene emissions have been believed to be from only photosynthesis processes in plant. However nocturnal isoprene emission from pine is detected. And by feeding 13CO2 to plants, it is found that both photosynthesis pathway and light independent processes contribute to isoprene emissions.
2002, 13(9): 901-902
Abstract:
The copolymer (EO)22(PO)52(EO)22 in p-xylene can solubilize much more water in the presence of compressed CO2 than the case without CO2.
The copolymer (EO)22(PO)52(EO)22 in p-xylene can solubilize much more water in the presence of compressed CO2 than the case without CO2.
2002, 13(9): 903-906
Abstract:
The breakthrough and stoichiometric SO2 adsorption efficiencies of a biomass supported Na2CO3 system (80 wt %Na2CO3/straw) have reached 48.9% and 80.6% respectively at a desulfurization temperature of 80℃.
The breakthrough and stoichiometric SO2 adsorption efficiencies of a biomass supported Na2CO3 system (80 wt %Na2CO3/straw) have reached 48.9% and 80.6% respectively at a desulfurization temperature of 80℃.
2002, 13(9): 907-910
Abstract:
The dynamic structure of Mo-O species in Ag-Mo-P-O catalyst was studied by in situ confocal microprobe laser Raman spectroscopy (LRS) and catalytic test. The results indicate Mo-O species of MoO3 transformed to Mo-O species of AgMoO2PO4 in C3H8/O2/N2 (3/1/4) flow at 773 K. This behavior is closely relative to oxidative dehydrogenation of propane and intrinsic properties of Mo-O species. The Mo-O species of AgMoO2PO4 may be active species for oxidative dehydrogenation of propane.
The dynamic structure of Mo-O species in Ag-Mo-P-O catalyst was studied by in situ confocal microprobe laser Raman spectroscopy (LRS) and catalytic test. The results indicate Mo-O species of MoO3 transformed to Mo-O species of AgMoO2PO4 in C3H8/O2/N2 (3/1/4) flow at 773 K. This behavior is closely relative to oxidative dehydrogenation of propane and intrinsic properties of Mo-O species. The Mo-O species of AgMoO2PO4 may be active species for oxidative dehydrogenation of propane.
2002, 13(9): 911-914
Abstract:
The toluene conversion, the selectivity to styrene and ethylbenzene (C8 selectivity) in the oxidative methylation of toluene with methane have been studied comparatively for the KY zeolite catalyst promoted with Li2O, Na2O, K2O, and Cs2O respectively. It was found that the effect of promoter decreased in the order:Cs2O > Na2O > Li2O > K2O.
The toluene conversion, the selectivity to styrene and ethylbenzene (C8 selectivity) in the oxidative methylation of toluene with methane have been studied comparatively for the KY zeolite catalyst promoted with Li2O, Na2O, K2O, and Cs2O respectively. It was found that the effect of promoter decreased in the order:Cs2O > Na2O > Li2O > K2O.
2002, 13(9): 915-918
Abstract:
A novel organic-inorganic complex [Ca(DMSO)5(H2O)]2SiMo12O40 was synthesized from CaCl2, DMSO and H4SiMo12O40·nH2O in mixed solvent of acetonitrile and water. Its structure was characterized with elemental analysis, IR and X-ray diffraction analysis.
A novel organic-inorganic complex [Ca(DMSO)5(H2O)]2SiMo12O40 was synthesized from CaCl2, DMSO and H4SiMo12O40·nH2O in mixed solvent of acetonitrile and water. Its structure was characterized with elemental analysis, IR and X-ray diffraction analysis.
