| 1-甲基-4-哌啶酮的合成 |
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| 引用本文： | 杨帆,陈立功,王东华. 1-甲基-4-哌啶酮的合成[J]. 精细化工, 2007, 24(11): 1142-1144 |
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| 作者姓名： | 杨帆 陈立功 王东华 |
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| 作者单位： | 天津大学,药物科学与技术学院,天津,300072;天津大学,药物科学与技术学院,天津,300072;天津大学,药物科学与技术学院,天津,300072 |
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| 摘 要： | 以甲胺的甲醇溶液和丙烯酸甲酯为原料,经Michael加成、Dieckmann环合和脱羧反应合成得到了1-甲基-4-哌啶酮,并对各步反应的工艺参数进行了优化,在n(丙烯酸甲酯)/n(甲胺)=2.2,n(甲醇钠)/n〔甲基-二-(β-甲氧羰乙基)胺〕=1.14,Michael加成反应温度25℃,Dieckmann环合反应温度80～83℃,脱羧反应温度100～103℃的条件下,1-甲基-4-哌啶酮的总收率为58%,并按该工艺顺利完成了500L反应釜中试。
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| 关 键 词： | 哌啶酮 迈克尔加成 狄克曼环合 脱羧 精细化工中间体 |
| 文章编号： | 1003-5214（2007）11-1142-03 |
| 修稿时间： | 2007-02-07 |
Synthesis of 1-Methyl-4-piperidone |
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| YANG Fan,CHEN Li-gong,WANG Dong-hua. Synthesis of 1-Methyl-4-piperidone[J]. Fine Chemicals, 2007, 24(11): 1142-1144 |
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| Authors: | YANG Fan CHEN Li-gong WANG Dong-hua |
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| Affiliation: | School of Pharmaceutical Science and Technology, Tianjin University, Tianjin 300072, China |
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| Abstract: | 1-Methyl-4-piperidone was obtained from a methanol solution of methylamine and methyl acrylate through Michael addition,Dieckmann cyclization and decarboxylation.Thus,with n(methyl acrylate)/n(methylamine)=2.2 and n(sodium methoxide)/nmethyl-di-(β-methoxycarbonylethyl)amine=1.14,Michael addition at 25 ℃,Dieckmann cyclization at 80～83 ℃ and decarboxylation at 100～103 ℃,the total yield of 1-methyl-4-piperidone was 58%.500 L reactor pilot test was successfully carried out. |
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| Keywords: | piperidone Michael addition Dieckmann cyclization decarboxylation fine chemicals intermediate |
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