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
By taking 3 chloro 4 methyl aniline as raw material,two solvent mixtures of naphtha and petroleum ether in a certain proportion,and through sulfonation 2 amino 4 chloro 5 toluene sulfonic acid was synthesized.The yiel...By taking 3 chloro 4 methyl aniline as raw material,two solvent mixtures of naphtha and petroleum ether in a certain proportion,and through sulfonation 2 amino 4 chloro 5 toluene sulfonic acid was synthesized.The yield of product was about 90%,and the recovery of solvents was over 95%.展开更多
The 3 (4 aminophenylazo)benzenesulfonic sodium and 3 (4 amino 3 methylphenylazo) benzenesulfonic sodium have been synthesized via protecting NH 2 group in aniline o toluidine by -CH 2SO 3Na and characterized by IR and...The 3 (4 aminophenylazo)benzenesulfonic sodium and 3 (4 amino 3 methylphenylazo) benzenesulfonic sodium have been synthesized via protecting NH 2 group in aniline o toluidine by -CH 2SO 3Na and characterized by IR and 13 C NMR.展开更多
The title compound 3 was synthesized from diethylguanidine nitrate（2） obtained from diethylamine, CaCN2 and HNO3. The mixture consisted of 0.5 mol 2, 0.55 mol acetonyl propionate, 3 g benzyltriethylammonium chloride...The title compound 3 was synthesized from diethylguanidine nitrate（2） obtained from diethylamine, CaCN2 and HNO3. The mixture consisted of 0.5 mol 2, 0.55 mol acetonyl propionate, 3 g benzyltriethylammonium chloride, and 44 g NaOH was refluxed for 4 hours to give 85 g 3, in yield 94.6%.展开更多
A series of 2 amimo 3 cyano 7,7 dimethyl 4 aryl 5 oxo 5,6,7,8 tetra 4H chromenes were synthesized in the absence of catalyst. Their structures were determined by IR, 1H NMR, and single crystal X ray diffraction.
以4-氨基-3-甲基苯甲酸为起始原料,经混酸硝化反应、正丁酸酐酰化反应和甲醇酯化反应等三步合成目标产物3-甲基-4-正丁酰氨基-5-硝基苯甲酸甲酯.其中间产物和目标产物的化学结构均经1 H NMR、13 C NMR、MS等方法进行了表征.实验过程中...以4-氨基-3-甲基苯甲酸为起始原料,经混酸硝化反应、正丁酸酐酰化反应和甲醇酯化反应等三步合成目标产物3-甲基-4-正丁酰氨基-5-硝基苯甲酸甲酯.其中间产物和目标产物的化学结构均经1 H NMR、13 C NMR、MS等方法进行了表征.实验过程中还对各步反应条件进行了优化,各步在最佳反应条件下总产率可达72.6%.该合成路线简单易行,容易实现工业化生产,具有很好的应用价值.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By taking 3 chloro 4 methyl aniline as raw material,two solvent mixtures of naphtha and petroleum ether in a certain proportion,and through sulfonation 2 amino 4 chloro 5 toluene sulfonic acid was synthesized.The yield of product was about 90%,and the recovery of solvents was over 95%.
文摘The 3 (4 aminophenylazo)benzenesulfonic sodium and 3 (4 amino 3 methylphenylazo) benzenesulfonic sodium have been synthesized via protecting NH 2 group in aniline o toluidine by -CH 2SO 3Na and characterized by IR and 13 C NMR.
文摘The title compound 3 was synthesized from diethylguanidine nitrate（2） obtained from diethylamine, CaCN2 and HNO3. The mixture consisted of 0.5 mol 2, 0.55 mol acetonyl propionate, 3 g benzyltriethylammonium chloride, and 44 g NaOH was refluxed for 4 hours to give 85 g 3, in yield 94.6%.
文摘A series of 2 amimo 3 cyano 7,7 dimethyl 4 aryl 5 oxo 5,6,7,8 tetra 4H chromenes were synthesized in the absence of catalyst. Their structures were determined by IR, 1H NMR, and single crystal X ray diffraction.
文摘以4-氨基-3-甲基苯甲酸为起始原料,经混酸硝化反应、正丁酸酐酰化反应和甲醇酯化反应等三步合成目标产物3-甲基-4-正丁酰氨基-5-硝基苯甲酸甲酯.其中间产物和目标产物的化学结构均经1 H NMR、13 C NMR、MS等方法进行了表征.实验过程中还对各步反应条件进行了优化,各步在最佳反应条件下总产率可达72.6%.该合成路线简单易行,容易实现工业化生产,具有很好的应用价值.
