摘要
以苯甲醚和丙烯腈为原料,经过F-C反应→水解→Hoffmann降解→脱甲基和精制成盐合成了对羟基苯乙胺盐酸盐。研究了不同反应条件对反应收率的影响,F-C反应中氯化氢的通入量对F-C反应收率影响很大,最佳值为通入时间2 h,流量0.5 L/min;Hoffmann降解反应中自制次氯酸钠比市售的效果好,反应温度70℃;脱甲基和精制过程中,需加入适量还原剂以阻止酚羟基的氧化;路线总收率达60%。
p-Hydroxyphenyl ethylamine hydrochloric salt was synthesized from benzyl methyl ether and acrylonitrile,through F-C reaction, hydrolyzation, Hoffmann reducing reaction, de-protect methyl group and refining. The effect of different reaction conditions on reaction yield. The amount of hydrochloric acid effect on the yield of F-C reaction, the best amount of hydrochloric acid is 0.5 L/min rate and 2 h. The sodium hypochlorite is more effective than the market sodium hypochlorite in Hoffmann reducing reaetion, the reaction temperature is 70 ℃. Reductive agent is used to prevent the oxidation of phenol hydroxyl group in de-protected and refining procedure. The total yield of route is 60%.
出处
《应用化工》
CAS
CSCD
2009年第5期763-765,共3页
Applied Chemical Industry
关键词
医药中间体
对羟基苯乙胺盐酸盐
反应条件
合成
精制
medicinal intermediate
p-hydroxyphenyl ethylamine hydrochloric salt
reaction condition
synthesis
refining
