Synthesis steps of 4,5 diamino 6 hydroxy 2 mercaptopyrimidine were improved on cyclocondensation of ethyl cyanoacetate with thiourea,nitrosation and reduction to obtain the product in 89% yield with high purity on ind...Synthesis steps of 4,5 diamino 6 hydroxy 2 mercaptopyrimidine were improved on cyclocondensation of ethyl cyanoacetate with thiourea,nitrosation and reduction to obtain the product in 89% yield with high purity on industrial scale.展开更多
以硫脲和氯乙酸为原料,在无溶剂和350 W微波辐射4 m in条件下,缩合生成中间体2,4-噻唑烷二酮(Ⅰ)产率91.5%;随后在无溶剂和400 W微波辐射5 m in条件下,通过V ilsm e ier甲酰化反应,生成中间体4-氯-5-甲酰基噻唑-2(3H)-酮(Ⅱ),产率86.7%...以硫脲和氯乙酸为原料,在无溶剂和350 W微波辐射4 m in条件下,缩合生成中间体2,4-噻唑烷二酮(Ⅰ)产率91.5%;随后在无溶剂和400 W微波辐射5 m in条件下,通过V ilsm e ier甲酰化反应,生成中间体4-氯-5-甲酰基噻唑-2(3H)-酮(Ⅱ),产率86.7%;最后以正丙醇为溶剂,450 W微波辐射7 m in条件下,成环得到5-氨基-噻唑[4,5-d]嘧啶-2(3H)-酮(Ⅲ),产率80.5%。反应总产率为63.9%。合成产物与中间体的结构经1HNMR,MS和元素分析确认。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
Ten N (4 substituted pyrimidin 2 yl) 2 trifluoroacetylamino benzenesulfonylureas were synthesized. Their structures were confirmed by elemental analysis and 1H NMR. Some of the compounds showed good herbicidal act...Ten N (4 substituted pyrimidin 2 yl) 2 trifluoroacetylamino benzenesulfonylureas were synthesized. Their structures were confirmed by elemental analysis and 1H NMR. Some of the compounds showed good herbicidal activity.展开更多
文摘Synthesis steps of 4,5 diamino 6 hydroxy 2 mercaptopyrimidine were improved on cyclocondensation of ethyl cyanoacetate with thiourea,nitrosation and reduction to obtain the product in 89% yield with high purity on industrial scale.
文摘以硫脲和氯乙酸为原料,在无溶剂和350 W微波辐射4 m in条件下,缩合生成中间体2,4-噻唑烷二酮(Ⅰ)产率91.5%;随后在无溶剂和400 W微波辐射5 m in条件下,通过V ilsm e ier甲酰化反应,生成中间体4-氯-5-甲酰基噻唑-2(3H)-酮(Ⅱ),产率86.7%;最后以正丙醇为溶剂,450 W微波辐射7 m in条件下,成环得到5-氨基-噻唑[4,5-d]嘧啶-2(3H)-酮(Ⅲ),产率80.5%。反应总产率为63.9%。合成产物与中间体的结构经1HNMR,MS和元素分析确认。
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Ten N (4 substituted pyrimidin 2 yl) 2 trifluoroacetylamino benzenesulfonylureas were synthesized. Their structures were confirmed by elemental analysis and 1H NMR. Some of the compounds showed good herbicidal activity.
