摘要
以氯乙烯和金属镁为原料,反应制得格氏试剂乙烯基氯化镁;再与β-紫罗兰酮发生加成反应得到合成维生素A的重要中间体乙烯基-β-紫罗兰醇。通过对反应条件和工艺的研究和优化,确定了最佳工艺条件为:金属镁与β-紫罗兰酮的摩尔比为1.3∶1.0,滴加β-紫罗兰酮的温度为0~5℃,在反应温度20~25℃时继续反应3~4h,得到乙烯基-β-紫罗兰醇的收率为98.0%,气相色谱(GC)分析含量为92.5%。该工艺条件得到了实验室放大的验证。
The Grinard reagent vinylmagnesium chloride was prepared from vinyl chloride and magnesium. The intermediate of Vitamin A vinyl-β-ionol was synthesized by the addition reaction of vinylmagnesium chloride with β-ionone. The optimal process was determined through the optimization and research of the reaction and process conditions. The yield of vinyl-β-ionol was 98.0% and the GC content was 92.5 % when molar ratio of metal magnesium and β-ionone was 1.3 : 1.0, dropping temperature was 0 - 5 ℃, and then reaction time continued for 3 - 4 h at the temperature of 20 - 25 ℃. The process was confirmed by lab amplification.
出处
《上海应用技术学院学报(自然科学版)》
2013年第3期186-188,200,共4页
Journal of Shanghai Institute of Technology: Natural Science
基金
上海应用技术学院引进人才基金资助项目(YJ2011-07)
上海应用技术学院大学生创新基金资助项目(DCXZ2011-06)