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。
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 )/n [ methyl-di- (β-methoxycarbonylethyl) amlne]= 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.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2007年第11期1142-1144,共3页
Fine Chemicals
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
piperidone
Michael addition
Dieckmann cyclization
decarboxylation
fine chemicals intermediate