期刊信息
- 刊名： 河北师范大学学报（自然科学版）Journal of Hebei Normal University (Natural Science)
- 主办： 河北师范大学
- ISSN： 1000-5854
- CN： 13-1061/N
- 中国科技核心期刊
- 中国期刊方阵入选期刊
- 中国高校优秀科技期刊
- 华北优秀期刊
- 河北省优秀科技期刊
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
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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 -
DOI：
The Synthesis of 2,2-dipheny1-2-hydroxyacetic Acid-1-methyl-4-piperidinyl Ester and Its Crystal Structure
摘要/Abstract
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1HNMR表征,并测定了其晶体结构.
The synthesis of 2,2-dipheny1-2-hydrox yacetic acid-1-methy1-4-piperidinyl ester(4) was studied,which was an important intermediate and metabolite of propiverine hydrochloride.Reaction of 2,2-dipheny1-2-hydrox yacetate with enough methanol gave methyl ester in 95% yield.Compound 4 was obtained by reaction of methyl 2,2-dipheny1-2-hy drox yacetate with 1-methy1-4-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 by1H NMR and crystal structure was determined.