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1996 Volume 7 Issue 6
1996, 7(6): 503-504
Abstract:
A new kind of coenzyme B12 analogue 2',3',5'-trideoxyuridinyl-cobalamin (ddUCbl) was first synthesized by an improved method in which 5'-O-toluenesulfonyl-2',3'-dideoxyuridine was first transformed into 5'-iodo-2',3'-dideoxyuridine and then reacted with reduced hydroxocobalamin.The new analogue was characterized by UV-vis and 1HNMR spectroscopy.
A new kind of coenzyme B12 analogue 2',3',5'-trideoxyuridinyl-cobalamin (ddUCbl) was first synthesized by an improved method in which 5'-O-toluenesulfonyl-2',3'-dideoxyuridine was first transformed into 5'-iodo-2',3'-dideoxyuridine and then reacted with reduced hydroxocobalamin.The new analogue was characterized by UV-vis and 1HNMR spectroscopy.
1996, 7(6): 505-506
Abstract:
Reaction of 3,7-dinitrodibenzobromolium bisulfate with some nucleophiles were studied.Primary products of reactions are 2-bromo-2'-Nu-4-4 '-dinitro-biphenyls.
Reaction of 3,7-dinitrodibenzobromolium bisulfate with some nucleophiles were studied.Primary products of reactions are 2-bromo-2'-Nu-4-4 '-dinitro-biphenyls.
1996, 7(6): 507-508
Abstract:
A rosmarinic acid derivative,tetramethyl ether of rosmarinic acid benzyl ester,was synthesized.This is the first report of building this structural skeleton.
A rosmarinic acid derivative,tetramethyl ether of rosmarinic acid benzyl ester,was synthesized.This is the first report of building this structural skeleton.
1996, 7(6): 509-510
Abstract:
New 3-oxo-benzoisothiazoline-2-acetamide 1,1- dioxides (Ila-b) were synthesized and whose reaction with alkoxides was studied.The reaction results indicated that different products were obtained owing to the different time of reaction with alkoxides.
New 3-oxo-benzoisothiazoline-2-acetamide 1,1- dioxides (Ila-b) were synthesized and whose reaction with alkoxides was studied.The reaction results indicated that different products were obtained owing to the different time of reaction with alkoxides.
1996, 7(6): 511-512
Abstract:
Treatment of 2,4,6,8,10,12-hexabenzyl-2,4,6,8,10,12-hexaazatetracyclo-[5.5.0.03.9.03.11]dodecane (1) with Me2CHNO2/CuCl/Py/O2 results in C (1)-C (7); oxidative cleavage to give 1,3.4,5,7,8-hexabenzyt-2,6-dioxo-cis-cisoid-cis-decahydro-1H,5H-diimidazo [4,5-b:4',5'-e] pyrazine (2).
Treatment of 2,4,6,8,10,12-hexabenzyl-2,4,6,8,10,12-hexaazatetracyclo-[5.5.0.03.9.03.11]dodecane (1) with Me2CHNO2/CuCl/Py/O2 results in C (1)-C (7); oxidative cleavage to give 1,3.4,5,7,8-hexabenzyt-2,6-dioxo-cis-cisoid-cis-decahydro-1H,5H-diimidazo [4,5-b:4',5'-e] pyrazine (2).
1996, 7(6): 513-514
Abstract:
The iodide form of anion exchange resins with quaternary ammonium could effectively catalyze the synthesis of propylene carbonate from carbon dioxide and propylene oxide in proper dipolar aprotic solvents.The resins could be reused for many runs without much loss of catalytic activity.
The iodide form of anion exchange resins with quaternary ammonium could effectively catalyze the synthesis of propylene carbonate from carbon dioxide and propylene oxide in proper dipolar aprotic solvents.The resins could be reused for many runs without much loss of catalytic activity.
1996, 7(6): 515-518
Abstract:
This paper reports the synthesis of selenacrown ethers with hydroxy group and disclenaaza-crown ethers.
This paper reports the synthesis of selenacrown ethers with hydroxy group and disclenaaza-crown ethers.
1996, 7(6): 519-522
Abstract:
Two types of effective transesterification catalysts including ordinary anion exchange resins and polymer-supported triphenyl phosphines are used to synthesize propylene glycol and dimethyl carbonate from propylene carbonate and methanol.The experimental results show that the products can be obtained under moderate conditions using these catalysts.Triphenyl phosphine polymeric catalysts are found thermally stable by thermogravimetry (TG).
Two types of effective transesterification catalysts including ordinary anion exchange resins and polymer-supported triphenyl phosphines are used to synthesize propylene glycol and dimethyl carbonate from propylene carbonate and methanol.The experimental results show that the products can be obtained under moderate conditions using these catalysts.Triphenyl phosphine polymeric catalysts are found thermally stable by thermogravimetry (TG).
1996, 7(6): 523-526
Abstract:
A novel β-cyclodextrin (β-CD) derivative (2) bearing a single 8-quinolyl moiety has been synthesized by a convenient method in 41.4% yield,and the compound was characterized by 1H-NMR,FT-IR spectra and elemental analysis,etc.The spectrophotometric titrations have been performed in buffered aqueous solution (pH=7.20) to give the complex stability constants (K) and Gibbs free energy changes (-△G·) for the 1:1 inclusion complexation of some amino acids guest molecules with host compound (2) and mono-(6-anilino)-β-cyclodextrin (1).
A novel β-cyclodextrin (β-CD) derivative (2) bearing a single 8-quinolyl moiety has been synthesized by a convenient method in 41.4% yield,and the compound was characterized by 1H-NMR,FT-IR spectra and elemental analysis,etc.The spectrophotometric titrations have been performed in buffered aqueous solution (pH=7.20) to give the complex stability constants (K) and Gibbs free energy changes (-△G·) for the 1:1 inclusion complexation of some amino acids guest molecules with host compound (2) and mono-(6-anilino)-β-cyclodextrin (1).
1996, 7(6): 527-530
Abstract:
A series of aryloxy-acetic acids were synthesized by the reaction of substituted phenols with chloroacetic acid under the condition of microwave irradiation and with solid base as a support.This method has the advantage of better yields,shorter reaction time,and convenience.
A series of aryloxy-acetic acids were synthesized by the reaction of substituted phenols with chloroacetic acid under the condition of microwave irradiation and with solid base as a support.This method has the advantage of better yields,shorter reaction time,and convenience.
1996, 7(6): 531-534
Abstract:
Cyclohexene was selectively oxidized with dioxygen by polyoxometalate intercalated layered double hydroxides to produce 2-cyclohexene-one and 2-cyclohexene-ol under mild reaction conditions.
Cyclohexene was selectively oxidized with dioxygen by polyoxometalate intercalated layered double hydroxides to produce 2-cyclohexene-one and 2-cyclohexene-ol under mild reaction conditions.
1996, 7(6): 535-538
Abstract:
Six kinds of new ditopic receptor macrocycles were synthesized by the condensation of 1,10-bis(4-formylphenyl)-1,4,7,10-tetraoxadecane or 1,10 —bis(4 —formyl-2-methoxyphenyl)-1,4,7,10-tetraoxadecane with polyamines.The macrocycles were characterized by elemental analysis,IR,1H NMR.
Six kinds of new ditopic receptor macrocycles were synthesized by the condensation of 1,10-bis(4-formylphenyl)-1,4,7,10-tetraoxadecane or 1,10 —bis(4 —formyl-2-methoxyphenyl)-1,4,7,10-tetraoxadecane with polyamines.The macrocycles were characterized by elemental analysis,IR,1H NMR.
1996, 7(6): 539-542
Abstract:
N',N'-bis(2-chloroethyl)-O-aryl-N3-ethoxycarbonyl substituted methylene ureido phosphoramidates (2) designed as promising antivirus and antitumor agents have been synthesized in excellent yields via the corresponding thiourea derivatives (1) involving a homogeneous desulphunsation reaction as the key step and the possible mechanism is proposed herein.The stability and cleavage of acid-catalyzed hydrolysis of 2 are also discussed.
N',N'-bis(2-chloroethyl)-O-aryl-N3-ethoxycarbonyl substituted methylene ureido phosphoramidates (2) designed as promising antivirus and antitumor agents have been synthesized in excellent yields via the corresponding thiourea derivatives (1) involving a homogeneous desulphunsation reaction as the key step and the possible mechanism is proposed herein.The stability and cleavage of acid-catalyzed hydrolysis of 2 are also discussed.
1996, 7(6): 543-544
Abstract:
2α,5α,10β,14β-Tetra-acetoxy-4(20),11-laxadiene (1) could be regioselectively transfonned into 6α,10β-dihydroxy-2α,5α,14β-triacetoxy-4(20),11-taxadiene (2) by Cunninghamella echinulata in fair yield.6β,10β-Dihydroxy-2α,5α,14β-triacetoxy-4(20),11-taxadiene (3).10β-bydroxy-2α,5α,14β- triacetoxy-4(20),11-taxadiene (4),10β-hydroxy-4β,20-epoxy-2α,5α,14β-triacetoxy-tax-11-ene (5) as minor products were also isolated.
2α,5α,10β,14β-Tetra-acetoxy-4(20),11-laxadiene (1) could be regioselectively transfonned into 6α,10β-dihydroxy-2α,5α,14β-triacetoxy-4(20),11-taxadiene (2) by Cunninghamella echinulata in fair yield.6β,10β-Dihydroxy-2α,5α,14β-triacetoxy-4(20),11-taxadiene (3).10β-bydroxy-2α,5α,14β- triacetoxy-4(20),11-taxadiene (4),10β-hydroxy-4β,20-epoxy-2α,5α,14β-triacetoxy-tax-11-ene (5) as minor products were also isolated.
1996, 7(6): 545-548
Abstract:
Cimicifugamide,a new natural compound isolated from the roots of Cimicifuga dahurica,was totally synthesized by a reaction sequence of seven steps in an overall yield of 31%.D-Galactose was used as starting material,trifluoroacetoxy was used as leaving group at C-1.The target product was characterized by IR,MS,1H-NMR,13C-NMR and elemental analysis.
Cimicifugamide,a new natural compound isolated from the roots of Cimicifuga dahurica,was totally synthesized by a reaction sequence of seven steps in an overall yield of 31%.D-Galactose was used as starting material,trifluoroacetoxy was used as leaving group at C-1.The target product was characterized by IR,MS,1H-NMR,13C-NMR and elemental analysis.
1996, 7(6): 549-552
Abstract:
Some derivatives of neo-clerodane diterpenes ajugacumbin A and B isolated from Ajuga decumbens were prepared by various chemical transformations,and the results achieved in the biological assay as insect antifeedants of these neo-clerodane derivatives are also reported.
Some derivatives of neo-clerodane diterpenes ajugacumbin A and B isolated from Ajuga decumbens were prepared by various chemical transformations,and the results achieved in the biological assay as insect antifeedants of these neo-clerodane derivatives are also reported.
1996, 7(6): 553-544
Abstract:
From the roots of Maackia temfolia,a new isoprenoid-substituted isoflavan was isolated and elucidated as Tenuifolin A (1)
From the roots of Maackia temfolia,a new isoprenoid-substituted isoflavan was isolated and elucidated as Tenuifolin A (1)
1996, 7(6): 555-556
Abstract:
A new lycoctonine-type norditerpenoid alkaloid,.omeienine 1,was isolated from the roots of Delphinium omeiense W.T.Wang.Its structure was elucidated by spectral methods.
A new lycoctonine-type norditerpenoid alkaloid,.omeienine 1,was isolated from the roots of Delphinium omeiense W.T.Wang.Its structure was elucidated by spectral methods.
1996, 7(6): 557-560
Abstract:
Two new diterpenoid alkaloids,tongoline (1) and tongolinine (2) were isolated from the whole plants of Delphinium tongolense F.,Their structures were determined on the basis of spectral data.
Two new diterpenoid alkaloids,tongoline (1) and tongolinine (2) were isolated from the whole plants of Delphinium tongolense F.,Their structures were determined on the basis of spectral data.
1996, 7(6): 561-564
Abstract:
Muricatalicin (2),a new acetogenin-(polyketide) has been isolated from the seed of Annona muricata L.Its structure and relative stereochemistry were elucidated on the basis of the spectral analysis.Muricatalicin (2) is a C35 mono-tetrahydrofuranyl (THF) acetogenin possessing five hydroxyl groups at C-4,C-7,C-13,C-15 and C-20.The relative configuration from C-15 through C-20 were determined as threo,trans and threo configuration.
Muricatalicin (2),a new acetogenin-(polyketide) has been isolated from the seed of Annona muricata L.Its structure and relative stereochemistry were elucidated on the basis of the spectral analysis.Muricatalicin (2) is a C35 mono-tetrahydrofuranyl (THF) acetogenin possessing five hydroxyl groups at C-4,C-7,C-13,C-15 and C-20.The relative configuration from C-15 through C-20 were determined as threo,trans and threo configuration.
1996, 7(6): 565-566
Abstract:
The present paper covers the synthesis and characterization of a mixed valence vanadate,(H2En) V4O10 (Compound I,H2En= H3NCH2CH2NH3),in which the VN/VN ratio is unity.The X-Ray diffraction pattern and DTA-TG curve are given.
The present paper covers the synthesis and characterization of a mixed valence vanadate,(H2En) V4O10 (Compound I,H2En= H3NCH2CH2NH3),in which the VN/VN ratio is unity.The X-Ray diffraction pattern and DTA-TG curve are given.
1996, 7(6): 567-568
Abstract:
The 1H and 13C NMR spectra of the dinuclear complexes of molybdenum (Ⅵ) with ethylenediaminetetraacetic acid ([Mo(VI)]2-EDTA) and 3,12-bis(carboxymethyl)-6,9-dioxa-3,12-diazatetra-decanedioic acid([Mo(VI)]2-EGTA) at various temperatures were measured.The solution structure of the two dinuclear complexes was determined and the possible exchange process of the isomers is suggested.
The 1H and 13C NMR spectra of the dinuclear complexes of molybdenum (Ⅵ) with ethylenediaminetetraacetic acid ([Mo(VI)]2-EDTA) and 3,12-bis(carboxymethyl)-6,9-dioxa-3,12-diazatetra-decanedioic acid([Mo(VI)]2-EGTA) at various temperatures were measured.The solution structure of the two dinuclear complexes was determined and the possible exchange process of the isomers is suggested.
1996, 7(6): 569-570
Abstract:
The structures of four isomeric forms of the model stannylenoid,H2SnLiF,have been examined by ab initio MO theory.The most stable structure is suggested to be the P-complex 1.The other three species,three-membered ring 2,σ-complex 3 and tetrahedron 4,are also local minima on the potential energy surface,but are higher in energy.
The structures of four isomeric forms of the model stannylenoid,H2SnLiF,have been examined by ab initio MO theory.The most stable structure is suggested to be the P-complex 1.The other three species,three-membered ring 2,σ-complex 3 and tetrahedron 4,are also local minima on the potential energy surface,but are higher in energy.
1996, 7(6): 571-572
Abstract:
A [70] fulleropyrrolidine was obtained by refluxing the mixture of C70 cyclohexanone and 2-aminoisobutyric acid in chlorobenzene under N2.
A [70] fulleropyrrolidine was obtained by refluxing the mixture of C70 cyclohexanone and 2-aminoisobutyric acid in chlorobenzene under N2.
1996, 7(6): 573-576
Abstract:
A new bisethyldithionetetrathiafulvalene (ET) derivative was synthesised.The cyclic voltammogram comparison of asymmetric hydromethyl bisethyldithionetetrathiafulvalene (HMET) and ET was made.The single crystal of charge transfer complex HMETIX was obtained and characterised.The conductivity of the single crystal was measured between room temperature and liquid nitrogen temperature.This single crystal is a semiconductor in the liquid nitrogen temperature range.
A new bisethyldithionetetrathiafulvalene (ET) derivative was synthesised.The cyclic voltammogram comparison of asymmetric hydromethyl bisethyldithionetetrathiafulvalene (HMET) and ET was made.The single crystal of charge transfer complex HMETIX was obtained and characterised.The conductivity of the single crystal was measured between room temperature and liquid nitrogen temperature.This single crystal is a semiconductor in the liquid nitrogen temperature range.
1996, 7(6): 577-578
Abstract:
The axial ligation properties of 2-benzenimidazolethiol-1 inked iron (Ⅲ) porphyrins are presented along with their ESR studies.
The axial ligation properties of 2-benzenimidazolethiol-1 inked iron (Ⅲ) porphyrins are presented along with their ESR studies.
1996, 7(6): 579-580
Abstract:
A new Belousov-Zhabotinskii oscillator in the malic acid-NaBrO3-H2SO4-[CuL] (ClO4)2 system,where L is 5,7,12.14-tetraethyl-7,14-dimethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene,is reported.
A new Belousov-Zhabotinskii oscillator in the malic acid-NaBrO3-H2SO4-[CuL] (ClO4)2 system,where L is 5,7,12.14-tetraethyl-7,14-dimethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene,is reported.
1996, 7(6): 581-584
Abstract:
The reaction of Ca with HN3 has been investigated theoretically by an ab initio MO method with electron correlation being taken into account by second-order MØLLER-PLESSET (MP2) perturbation theory Two possible product channels,CaN3+H,CaNH+N2,on the potential energy surfaces (PESs) have been examined and the reaction mechanism discussed.Values of the HN-N2 ,H- N3,Ca-N3 and Ca-NH bond dissociation energy are also calculated,which are in good agreement with experiment.
The reaction of Ca with HN3 has been investigated theoretically by an ab initio MO method with electron correlation being taken into account by second-order MØLLER-PLESSET (MP2) perturbation theory Two possible product channels,CaN3+H,CaNH+N2,on the potential energy surfaces (PESs) have been examined and the reaction mechanism discussed.Values of the HN-N2 ,H- N3,Ca-N3 and Ca-NH bond dissociation energy are also calculated,which are in good agreement with experiment.
1996, 7(6): 585-588
Abstract:
A novel synthetic method for the clusters FeCo2(CO)9(RCCR)(R=MeO2C,MeO2C),which is the reaction of Co4(CO)10(RCCR) with Na2[Fe(CO)4],have been found by studying on the thermal reaction between RCCo3(CO)9 with Na2[Fe(CO)4].X-ray crystal structural determinations have been made for the clusters FeCo2(CO)9(MeO2CCCCO2Me) and Co4(CO)10(EtO2CCCCO2Et).
A novel synthetic method for the clusters FeCo2(CO)9(RCCR)(R=MeO2C,MeO2C),which is the reaction of Co4(CO)10(RCCR) with Na2[Fe(CO)4],have been found by studying on the thermal reaction between RCCo3(CO)9 with Na2[Fe(CO)4].X-ray crystal structural determinations have been made for the clusters FeCo2(CO)9(MeO2CCCCO2Me) and Co4(CO)10(EtO2CCCCO2Et).
1996, 7(6): 589-592
Abstract:
A convenient approach based on transesterification to preparing the complexes of β-alkoxycarbonylethyltin trichlorides with dibenzylsulfoxide (DBSO) and hexamethylphosphoramide (HMPA) was reported.The structures of complexes were characterized by elemental analysis,IR,1HNMR and X-ray single crystal diffraction.The possible mechanism for the transesterification of complexes of β-methoxycarb-onylethyltin trichloride with an alcohol was suggested.
A convenient approach based on transesterification to preparing the complexes of β-alkoxycarbonylethyltin trichlorides with dibenzylsulfoxide (DBSO) and hexamethylphosphoramide (HMPA) was reported.The structures of complexes were characterized by elemental analysis,IR,1HNMR and X-ray single crystal diffraction.The possible mechanism for the transesterification of complexes of β-methoxycarb-onylethyltin trichloride with an alcohol was suggested.
1996, 7(6): 593-596
Abstract:
The fluorescence system Sm-BID-CTAB has been discovered and its fluorescence characteristics have been studied.The excitation and emission wavelengths are 360 nm and 650 nm,respectively.The fluorescence intensity is a linear function of the concentration of samarium in the range 5.0×10-5-2.0×10-7mol/L.The detection limit is 5.0×10-9 mol/L.Standard addition method is used for the determination of samarium in synthetic rare earth sample with satisfactory results.
The fluorescence system Sm-BID-CTAB has been discovered and its fluorescence characteristics have been studied.The excitation and emission wavelengths are 360 nm and 650 nm,respectively.The fluorescence intensity is a linear function of the concentration of samarium in the range 5.0×10-5-2.0×10-7mol/L.The detection limit is 5.0×10-9 mol/L.Standard addition method is used for the determination of samarium in synthetic rare earth sample with satisfactory results.
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