百草枯催吐剂三氮唑嘧啶酮的合成

Synthesis of Paraquat Emetic-Amino Propyl Triazolo Tyrimidone(PP796)

甲基丙烯酸甲酯经溴化加成、醚化、催化裂化得3-甲氧基-2-甲基丙烯酸甲酯;单氰胺与二硫化碳在碱性条件下缩合、甲基化得氰亚胺基二硫代碳酸二甲酯,后与正丙胺缩合再与水合肼环合得氨基正丙胺基三氮唑,与苯甲醛醛缩合得醛缩物,再在缚酸剂下与3-甲氧基-2-甲基丙烯酸甲酯催化闭环后在盐酸中水解、去醛基得目标物。选择cat1#/2#为裂解和闭环催化剂,反应总收率达55.4%,产品纯度99.5%。

The technological method of the preparation of amino propyl triazolo pyrimidone from Methyl-3-methoxy-2-methylpropenoate and N-Cyanoimido-S,S-dimethyl-dithiocarbonate under the condition of existing cat1#、cat2# composite catalyst and soda as acid-captor was presented. The effect of catalyst acid-captor and PH control on the reaction was discussed.According to the result analysis and the data comparison,the best synthesize condition was determined, overall yield reached 55.4%,puyity:99.5%.