摘要
以异戊醛,吗啉和丙烯腈为原料,用一锅法合成了5-甲基-4-甲酰基-己腈。通过正交试验确定了最佳的反应条件:异戊醛0.1mol,n(异戊醛)∶n(吗啉)∶n(丙烯腈)=1.0∶1.2∶1.4;溶剂[V(甲醇)∶V(水)=18∶2]200mL·mol-1(以烯胺计),于70℃反应15h(第2步),产率96.06%,产物易分离和纯化。
5-Methyl-4-formacylhexanenitrile was synthesized from isovaleraldehyde, morpholine and acrylonitrile by one-pot reaction. The optimum reaction conditions were studied by orthogonal test (L_9 (3~4).) The isovaleraldehyde was 0.1 mol, n(isovaleraldehyde) ∶n(morpholine) ∶n(acrylonitrile)=1.0 ∶1.2 ∶(1.4), solvent[V(methanol) ∶V(water)=18 ∶2] was 200 mL·mol^(-1)(enamine), temperature was 70 ℃ and the reaction time was 15 h(second step). Under the optimal conditions, the yield was 96.06% and the product can be easily separated and purified.
出处
《合成化学》
CAS
CSCD
2005年第4期414-416,共3页
Chinese Journal of Synthetic Chemistry
关键词
异戊醛
吗啉
丙烯腈
正交实验
一锅合成
isovaleraldehyde
morpholine
acrylonitrile
solvent
orthogonal experiment
one-pot synthesis
