摘要
该文以(S)-1-苯乙胺、丙烯酸甲酯为原料,经Michael加成,Dieckmann环合,脱羧,合成了(S)-1-(1-苯基乙基)-4-哌啶酮。并对所涉及的Michael加成反应的工艺参数进行了优化。当(S)-1-苯乙胺与丙烯酸甲酯的摩尔比为1∶2.5,40℃反应10h,收率为92.4%,总收率为89.3%。目标产物及中间体的结构经核磁共振波谱进行了表征。
(S) -1-(1-Phenylethyl) -4-piperidone( I ) was prepared from (S) -1-phenylethylamine and methyl acrylate through Michael addition, Dieckmann cyclization and decarboxylation. Technological parameters involved in Michael addition were optimized. Thus, (S) -1-phenylethylamine reacted with methyl acrylate in mole ratio 1:2.5 under 40 ℃ for 10 h to give the intermediate in 92.4% yield, and the total yield of I was 89.3%. Structures of the title compound and the intermediate were confirmed by ^1HNMR and ^13CNMR.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2007年第11期1109-1111,共3页
Fine Chemicals