| 7-氯-2-氧代庚酸乙酯合成新方法 |
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| 引用本文： | 李军章. 7-氯-2-氧代庚酸乙酯合成新方法[J]. 精细化工, 2012, 29(11) |
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| 作者姓名： | 李军章 |
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| 作者单位： | 河北科技大学 |
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| 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。探讨了第一步反应和第二步反应的影响因素，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。
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| 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 |
| 收稿时间： | 2012-07-20 |
| 修稿时间： | 2012-09-03 |
New Method for the Synthesis of Ethyl 7-Chloro-2-oxoheptanoate |
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| LI Jun-zhang. New Method for the Synthesis of Ethyl 7-Chloro-2-oxoheptanoate[J]. Fine Chemicals, 2012, 29(11) |
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| Authors: | LI Jun-zhang |
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| Affiliation: | Hebei University of Science and Thechnology |
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| Abstract: | Ethyl 7-chloro-2-oxoheptanoate is an important intermidiate of cilastatin. Using macronano-K2CO3 as base, 2-(5-chloropentyl)malonate was synthesized from 1-bromo-5-chloropentane and diethyl malonate in anhydrous EtOH, and then it was oxided by air catalized by Cu(NO3)2.3H2O in CH3CN to give ethyl 7-chloro-2-oxoheptanoate. The influence factors of the first-step reaction and the second-step reaction were investigated. The optimaized overall yield was 90.2%. The target product was characterized by means of 1HNMR and 13CNMR. |
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| Keywords: | ethyl 7-chloro-2-oxoheptanoate micronano-K2CO3 diethyl maloate catalytic oxidation |
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