多果定的合成新工艺

New Synthetic Process of Dodinz

通过选择盐酸胍和氯代十二烷为原料,两步反应制得标题化合物,并确定最佳合成工艺是以无水乙醇为溶剂、盐酸胍和氯代十二烷用量分别为0.1 mol和0.15 mol、回流反应10 h。冷却析出产物,甲苯重结晶得中间体;再以甲苯为溶剂,滴加20%氢氧化钠溶液中和该中间体,接着与冰醋酸成盐制得,HPLC含量为98.0%,收率为95.1%。

In this work,guanidine hydrochloride and chlorinated dodecane areselected as raw materials,and the optimum synthesis process was determined by two-step reaction.Use anhydrous ethanol as solvent,mix guanidine hydrochloride（0. 1 mol） and chlorinated dodecane（0. 15 mol）,after refluxing and stirring for 10 h,the mixture was cooled to give the intermediate and recrystallized by toluene.Take toluene as solvent,drop the 20% sodium hydroxide solution to neutralize the intermediate,then form the salt with acetic acid.HPLC content is 98. 0% and the yield of 95. 1%.