吡贝地尔的合成工艺研究

Improved synthesis of piribedil

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。

Aim To improve the procedure of piribedil.Methods The intermediate piperonyl chloride（3） was obtained through cyclization and Blanc reaction by using o-dihydroxybenzene and dichloromethane as starting material.Another intermediate 1-（2-pyrimidyl）piperazine（4） was obtained through N-alkylation by using 2-chloropyrimidine and piperazine as starting material.After N-alkylation between intermediates（3） and（4）,piribedil could be obtained.Results and conclusion The structure of piribedil was confirmed by 1H-NMR,GC-MS.The overall yield is 44.2%.The improved process has the advantage of low cost and it is also suitable for industrial production.