Grignard reagents were prepared from the starting materials 1-bromo-3,5-difluorobenzene,1-bromo-2,4-difluorobenzene andbromo-3,4-difluorobenzene respectively,then reacted with diethyl carbonate to form magnesium tris(...Grignard reagents were prepared from the starting materials 1-bromo-3,5-difluorobenzene,1-bromo-2,4-difluorobenzene andbromo-3,4-difluorobenzene respectively,then reacted with diethyl carbonate to form magnesium tris(difluoropheny)methanol,and methacryloyl chloride was added dropwise to abtain tris(difluorophenyl)methyl methacrylates.The target products were synthesized in high overall yield(67～74%)with"one-pot"method.Structures of the compounds were comfirmed by IR,1HNMR,13CNMR and elemental analysis,and methanolysis was also studied.展开更多
The fused triazole derivatives,which is an important inhibitors of the dipeptidyl peptidase-Ⅳ enzyme(DPP-Ⅳ),can be used for the treatment or prevention of type 2 diabetes.A new fused triazole derivatives of 3-oxo-3-...The fused triazole derivatives,which is an important inhibitors of the dipeptidyl peptidase-Ⅳ enzyme(DPP-Ⅳ),can be used for the treatment or prevention of type 2 diabetes.A new fused triazole derivatives of 3-oxo-3-[3-trifluoromethyl-5,6-dihydro[1,2,4]-triazolo[4,3-a]pyrazin-7(8H)-yl]-1-phenylpropan-1-amine was synthesized from 2-chloropyrazine and benzaldehyde by hydrazinolysis,trifluoroacetylation,cyclization,hydrogenation,condensation and deprotection reaction.The structures of the compound and its intermediates were determined by IR,NMR,and MS.展开更多
In this report the synthesis and characterization of chiral stationary phase of cellulose tris(3,5 dimethylphenylcarbamate) coated zirconia(CDMPC ZrO 2 CSP) was described. Direct optical resolutions of acidic racemate...In this report the synthesis and characterization of chiral stationary phase of cellulose tris(3,5 dimethylphenylcarbamate) coated zirconia(CDMPC ZrO 2 CSP) was described. Direct optical resolutions of acidic racemate naproxen and its derivatives on the phase were investigated. Surface property of zirconia affects the chiral separation of naproxen greatly. Naproxen could not be eluted from the column unless an acidic modifier was present in the mobile phase. However, good chiral resolutions were obtained for its ester derivatives. The influences of loading amount of stationary phase, molecular structure of compounds, type of alcohols as the modifier and their concentration in mobile phase on chiral resolution were studied. The chiral recognition mechanism of the chiral stationary phase was discussed.展开更多
基金supported by the "111 Project" from the Ministry of Education of China and the State Administration of Foreign Expert Affairs of China(No.111-2-07)National Science and Technology Major Projects of China(No.2012ZX09103-101-030)and the Project Program of State Key Laboratory of Natural Medicines,China Pharmaceutical University(No.ZJ12009)
文摘Grignard reagents were prepared from the starting materials 1-bromo-3,5-difluorobenzene,1-bromo-2,4-difluorobenzene andbromo-3,4-difluorobenzene respectively,then reacted with diethyl carbonate to form magnesium tris(difluoropheny)methanol,and methacryloyl chloride was added dropwise to abtain tris(difluorophenyl)methyl methacrylates.The target products were synthesized in high overall yield(67～74%)with"one-pot"method.Structures of the compounds were comfirmed by IR,1HNMR,13CNMR and elemental analysis,and methanolysis was also studied.
文摘The fused triazole derivatives,which is an important inhibitors of the dipeptidyl peptidase-Ⅳ enzyme(DPP-Ⅳ),can be used for the treatment or prevention of type 2 diabetes.A new fused triazole derivatives of 3-oxo-3-[3-trifluoromethyl-5,6-dihydro[1,2,4]-triazolo[4,3-a]pyrazin-7(8H)-yl]-1-phenylpropan-1-amine was synthesized from 2-chloropyrazine and benzaldehyde by hydrazinolysis,trifluoroacetylation,cyclization,hydrogenation,condensation and deprotection reaction.The structures of the compound and its intermediates were determined by IR,NMR,and MS.
文摘In this report the synthesis and characterization of chiral stationary phase of cellulose tris(3,5 dimethylphenylcarbamate) coated zirconia(CDMPC ZrO 2 CSP) was described. Direct optical resolutions of acidic racemate naproxen and its derivatives on the phase were investigated. Surface property of zirconia affects the chiral separation of naproxen greatly. Naproxen could not be eluted from the column unless an acidic modifier was present in the mobile phase. However, good chiral resolutions were obtained for its ester derivatives. The influences of loading amount of stationary phase, molecular structure of compounds, type of alcohols as the modifier and their concentration in mobile phase on chiral resolution were studied. The chiral recognition mechanism of the chiral stationary phase was discussed.
