摘要
以乙酰乙酸乙酯为原料合成氮杂螺环(8),对其合成工艺中的三元环化反应进行了改进,采用γ-环糊精作相转移催化剂,使得该步反应时间缩短至5 h,收率提高至96.8%。考察该反应条件,得出最佳的工艺条件:γ-环糊精作相转移催化剂,n(γ-环糊精)∶n(4)=0.1,最佳反应温度70℃,反应时间5 h。回收γ-环糊精,并讨论其再利用效果。改进后的工艺更加经济高效。
The aza spiro alkane (8) has been prepared from ethylacetoacetate. The reaction of cyclization in the process of aza spiro alkane has been improved. y-CD was used as the phase transfer catalyst making the reaction time shortened to 5 h and the yield up to 96.8 %. Comparing to the reaction conditions, optimal conditions were that: y-CD was used as phase transfer catalyst, n(y-CD) : n(4)-0.1, the best reaction temperature was 70 ℃ reaction time was 6 h. The effect of recycled 3,-CD on cyclization was discussed. The improved method was more economical and efficient.
出处
《广东化工》
CAS
2015年第18期7-8,共2页
Guangdong Chemical Industry
关键词
氮杂螺环
环化
Γ-环糊精
相转移催化剂
回收
aza spiro alkane;cyclization;y-CD;phase transfer catalyst;recycling