2,2-二苯基-2-羟基乙酸-1-甲基-4-哌啶醇酯的合成及晶体结构  

The Synthesis of 2,2-diphenyl-2-hydroxyacetic Acid-1-methyl-4-piperidinyl Ester and Its Crystal Structure

作　　者：刘倩[1] 吴桂叶[2] 陈金萍[1] 张静[1] 贾景景[1] 于奕峰[1] 付德才[1] 

机构地区：[1]河北科技大学化学与制药工程学院,河北石家庄050018 [2]大连理工大学化工学院,辽宁大连116023

出　　处：《河北师范大学学报（自然科学版）》2008年第5期646-648,共3页Journal of Hebei Normal University：Natural Science

基　　金：河北金通医药化工有限公司资助项目

摘　　要：研究了盐酸丙哌维林重要中间体及代谢产物2,2-二苯基-2-羟基乙酸-1-甲基-4-哌啶醇酯(4)的合成方法.2,2-二苯基-2-羟基乙酸与足量甲醇经酯化反应,以95%的收率得到2,2-二苯基-2-羟基乙酸甲酯,在金属钠的存在下,以甲苯和甲醇混合物为溶剂,与1-甲基-4-哌啶醇进行酯交换反应制备化合物4,高效液相色谱测得其质量分数>99.0%,收率达84.6%.产品经1H NMR表征,并测定了其晶体结构.The synthesis of 2,2-diphenyl-2-hydroxyacetic acid-1-methyl-4-plperidinyl ester （4） was studied, which was an important intermediate and metabolite of propiverine hydrochloride. Reaction of 2,2-diphenyl-2- hydroxyacetate with enough methanol gave methyl ester in 95 % yield. Compound 4 was obtained by reaction of methyl 2,2-diphenyl-2-hydroxyacetate with 1-methyl-4-piperidinol in the mixture of toluene and methanol in the presence of metal sodium. The yield was 84.6 % and the purity of the product was higher than 99.0 % （HPLC）. The chemical structure was confirmed by IH NMR and crystal structure was determined.

关 键 词：2 2-二苯基-2-羟基乙酸-1-甲基-4-哌啶醇酯 盐酸丙哌维林 合成 晶体结构 

分 类 号：O621.3[理学—有机化学]