摘要
以甘氨酸和丙烯腈为原料,经过迈克尔加成反应、酯化反应、氨基保护以及Dieckmann环合等4步反应,制备了1-Boc-3-氰基-4-吡咯烷酮,总收率66.4%。对关键的Michael加成和Dieckmann环合反应条件进行了优化,得到较佳反应条件:①迈克尔加成反应:丙烯腈与甘氨酸的摩尔比为1.1∶1,反应温度30℃,反应时间12 h;②环化反应:以甲苯为溶剂,1.3 mol的甲醇钠作碱,反应温度80℃,反应时间2 h。
1-Boc-3-cyano-4-oxopyrrolidine was synthesized from the starting material of glyeine nitrile by the reaction of Michael addition, esterification and Dieckmann cycltzation with the and aerylo- total yield 66.4%. The optimized reaction conditions of Michael addition and Dieckmann cyclization were Michael addition : acrylonitrile: glycine = mann cyclization : toluene as solvent, 1.3 1. 1: 1, reaction temperature 30℃, reaction time 12 tool NaOMe, reaction temperature 80 ℃, reaction time obtained: h ; Dieck- 2h.
出处
《应用化工》
CAS
CSCD
2013年第6期1081-1083,1088,共4页
Applied Chemical Industry