3,4-Dihydropyrimidin-2-(1H)-ones were synthesized in high yields by a one-pot cyclocondensation of aldehyde,1,3-dicarbonyl compound,and urea or thiourea using copper o-toluenesulfonate as a catalyst under solvent-free...3,4-Dihydropyrimidin-2-(1H)-ones were synthesized in high yields by a one-pot cyclocondensation of aldehyde,1,3-dicarbonyl compound,and urea or thiourea using copper o-toluenesulfonate as a catalyst under solvent-free conditions at 90℃.Effects of molar ratio of reactants,amount of catalyst,and reaction temperature on the yields of 3,4-dihydropyrimidin-2-(1H)-ones were investigated.The results showed that at the condition of naldehyde∶n1,3-dicarbonyl compounds∶nurea(or thiourea)=1∶1.2∶1.5,1 mol% catalyst(molar percent of aldehyde),2.0 h at 90℃,the yields of products were 51-96%.After reaction,the catalyst could be reused for four times without distinct loss of catalytic activity.展开更多
1-氧基磷杂-4-羟甲基-2,6,7-三氧杂双环[2.2.2]辛烷(PEPA)与三甲基氯硅烷反应合成阻燃成炭剂笼状1-氧基磷杂-4-三甲基硅氧甲基-2,6,7-三氧杂双环[2.2.2]辛烷酯(PTSPA)。探讨了不同溶剂、反应温度和反应物配比对产物产率的影响,最佳反应...1-氧基磷杂-4-羟甲基-2,6,7-三氧杂双环[2.2.2]辛烷(PEPA)与三甲基氯硅烷反应合成阻燃成炭剂笼状1-氧基磷杂-4-三甲基硅氧甲基-2,6,7-三氧杂双环[2.2.2]辛烷酯(PTSPA)。探讨了不同溶剂、反应温度和反应物配比对产物产率的影响,最佳反应条件是以二氧六环为溶剂,三乙胺为缚酸剂,PEPA与三甲基氯硅烷的物质的量比为1∶1.15,95℃反应8h,产率为91.6%。通过FT IR、1 H NMR、元素分析、极限氧指数及差热分析等技术表征了产物的结构及性能。实验表明,目标产物有较好的阻燃成炭性和热稳定性。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
文摘3,4-Dihydropyrimidin-2-(1H)-ones were synthesized in high yields by a one-pot cyclocondensation of aldehyde,1,3-dicarbonyl compound,and urea or thiourea using copper o-toluenesulfonate as a catalyst under solvent-free conditions at 90℃.Effects of molar ratio of reactants,amount of catalyst,and reaction temperature on the yields of 3,4-dihydropyrimidin-2-(1H)-ones were investigated.The results showed that at the condition of naldehyde∶n1,3-dicarbonyl compounds∶nurea(or thiourea)=1∶1.2∶1.5,1 mol% catalyst(molar percent of aldehyde),2.0 h at 90℃,the yields of products were 51-96%.After reaction,the catalyst could be reused for four times without distinct loss of catalytic activity.
文摘1-氧基磷杂-4-羟甲基-2,6,7-三氧杂双环[2.2.2]辛烷(PEPA)与三甲基氯硅烷反应合成阻燃成炭剂笼状1-氧基磷杂-4-三甲基硅氧甲基-2,6,7-三氧杂双环[2.2.2]辛烷酯(PTSPA)。探讨了不同溶剂、反应温度和反应物配比对产物产率的影响,最佳反应条件是以二氧六环为溶剂,三乙胺为缚酸剂,PEPA与三甲基氯硅烷的物质的量比为1∶1.15,95℃反应8h,产率为91.6%。通过FT IR、1 H NMR、元素分析、极限氧指数及差热分析等技术表征了产物的结构及性能。实验表明,目标产物有较好的阻燃成炭性和热稳定性。
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.
