烯酰吗啉合成新工艺研究
Study on a new synthesis process of enoylmorpholine
曾著飞 1徐志伟 1王峰 1刘天昆 1孙月 1胡国胜2
作者信息
- 1. 内蒙古冠仕达化学有限公司,内蒙古阿拉善 750306
- 2. 河北康辰制药有限公司,河北沧州 061162
- 折叠
摘要
为降低烯酰吗啉合成过程中N-乙酰吗啉的消耗,降低生产成本,在反应过程中加入了缚碱剂,以减少N-乙酰吗啉的分解.以4-氯-3',4'-二甲氧基二苯甲酮(E-苯酮)和N-乙酰吗啉为原料,二甲苯为溶剂,N,N-二甲基甲酰胺为缚碱剂,在叔丁醇钠催化作用下合成了烯酰吗啉.考察了投料比、反应温度、反应时间等因素对合成的影响,优化的反应条件为n(E-苯酮)∶n(N-乙酰吗啉)∶n(叔丁醇钠)∶n(N,N-二甲基甲酰胺)=1.00∶1.05∶1.15∶1.25,反应温度为 135℃,反应时间为 10 h,在此条件下产品烯酰吗啉收率 90.8%,纯度 97.6%.
Abstract
To reduce the consumption of N-acetylmorpholine in the synthesis process of enoylmorpholine and lower production costs,a base binding agent was added during the re-action to reduce the decomposition of N-acetylmorpholine.Enoylmorpholine was synthesized using 4-chloro-3',4'-dimethoxybenzophenone(E-phenyl ketone)and N-acetylmorpho-line as raw materials,xylene as solvent,and N,N-dimethylformamide as a base binding a-gent under the catalysis of sodium tert butanol.The influence of factors such as feed ratio,reaction temperature,and reaction time on the synthesis was investigated.The optimized re-action conditions were as follows,n(E-phenyl ketone)∶n(N-acetylmorpholine)∶n(sodium tert butanol)∶n(N,N-dimethylformamide)=1.00∶1.05∶1.15∶1.25,reaction temperature was 135℃,and reaction time was 10 hours.Under these conditions,the yield of the product enoylmor-pholine was 90.8%,and the purity was 97.6%.
关键词
烯酰吗啉/缚碱剂/N,N-二甲基甲酰胺/N-乙酰吗啉Key words
enoylmorpholine/alkaline binding agent/N,N-dimethylformamide/N-acetyl-morpholine引用本文复制引用
出版年
2024
NETL
NSTL
万方数据