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目的改进吡贝地尔的合成工艺。方法以邻苯二酚和二氯甲烷为原料经环和反应合成胡椒环,胡椒环与多聚甲醛经Blanc氯甲基化反应合成重要中间体胡椒基氯(3);以哌嗪和二氯嘧啶为原料经氮烷基化反应合成重要中间体1-(2-嘧啶基)哌嗪(4);3和4经氮烷基化反应得到目标化合物。结果与结论目标化合物的结构经1H-NMR、GC-MS谱确证,总收率为44.2%,改进后的工艺操作简便,成本低廉,有利于工业化生产。
Objective To improve the synthesis of piribedil. Methods Pepper rings were synthesized by ring reaction with catechol and methylene chloride. The key intermediate of piperonyl chloride (3) was synthesized by Blanc chloromethylation of pepper ring and paraformaldehyde. Piperazine and dichloro Pyrimidine as the starting material to synthesize the important intermediate 1- (2-pyrimidinyl) piperazine (4) via nitrogen alkylation; 3 and 4 were alkylated to obtain the target compound. Results and Conclusions The structure of the target compound was confirmed by 1H-NMR and GC-MS. The overall yield was 44.2%. The improved process was simple and easy to operate with low cost and was favorable for industrial production.