| 7-氯-2-氧代庚酸乙酯的合成 |
| |
| 引用本文： | 李军章,王家喜,刘守信. 7-氯-2-氧代庚酸乙酯的合成[J]. 精细化工, 2012, 0(11): 1084-1087,1092 |
| |
| 作者姓名： | 李军章 王家喜 刘守信 |
| |
| 作者单位： | 河北工业大学化工学院;河北科技大学化学与制药工程学院;河北省药物化工工程技术研究中心 |
| |
| 摘 要： | 7-氯-2-氧代庚酸乙酯是合成西司他丁的重要中间体。以微纳米碳酸钾为碱,1-溴-5-氯戊烷和丙二酸二乙酯在无水乙醇中反应得到2-(5-氯戊基)丙二酸二乙酯,然后在乙腈中三水硝酸铜催化下经空气氧化得到7-氯-2-氧代庚酸乙酯。探讨了第1步反应和第2步反应的影响因素,优化后两步反应总收率为90.2%。化合物的结构通过1HNMR和13CNMR进行了表征。
|
| 关 键 词： | 7-氯-2-氧代庚酸乙酯 微纳米碳酸钾 丙二酸二乙酯 催化氧化 医药原料 |
Synthesis of Ethyl 7-Chloro-2-oxoheptanoate |
| |
| LI Jun-zhang,WANG Jia-xi,LIU Shou-xin. Synthesis of Ethyl 7-Chloro-2-oxoheptanoate[J]. Fine Chemicals, 2012, 0(11): 1084-1087,1092 |
| |
| Authors: | LI Jun-zhang WANG Jia-xi LIU Shou-xin |
| |
| Affiliation: | 2,3(1.College of Chemical Engineering,Hebei University of Technology,Tianjin 030013,China;2.College of Chemical and Pharmaceutical Engineering,Hebi University of Science and Technology,Shijiazhuang 050071,Hebei,China;3.Hebei Research Center of Pharmaceutical and Chemical Engineering,Shijiazhuang 050071,Hebei,China) |
| |
| Abstract: | Ethyl 7-chloro-2-oxoheptanoate is an important intermediate in the synthesis of cilastatin.Using micronano-K2CO3 as base,diethyl 2-(5-chloropentyl)malonate was synthesized from 1-bromo-5-chloropentane and diethyl malonate in anhydrous EtOH,and then it was oxidized by air catalyzed by Cu(NO3)2·3H2O in CH3CN to give ethyl 7-chloro-2-oxoheptanoate.The influencing factors in the first-step reaction and the second-step reaction were investigated.The optimized overall yield was 90.2%.The target product was characterized by means of 1HNMR and 13CNMR. |
| |
| Keywords: | ethyl 7-chloro-2-oxoheptanoate micronano-K2CO3 diethyl malonate catalytic oxidation drug materials |
| 本文献已被 CNKI 等数据库收录！ |
|
