摘要
设计了1种合成盐酸甲氧那明的新工艺,以邻羟基苯乙酸为起始原料,经甲基化、Dakin-West反应、甲胺缩合成盐得到盐酸甲氧那明;考察了该工艺中催化剂、投料比、重结晶溶剂对反应收率和产品质量的影响。结果表明,在中间体邻甲氧基苯丙酮的制备中,邻羟基苯乙酸、硫酸二甲酯、氢氧化钠、醋酐、N-甲基咪唑的较佳投料摩尔比为1:2.5:4.0:2.5:0.2,在邻甲氧基苯丙甲胺的制备中,邻甲氧基苯丙酮、质量分数33%的甲胺乙醇溶液、Pt/C的较佳投料质量比为1:0.6:0.01,重结晶溶剂甲苯、乙醇质量比优选为5:1,总收率为46.5%(以邻羟基苯乙酸计算)。该工艺具有工业化前景。
A new process for the preparation of methoxyphenamine hydrochloride was designed.Methoxyphenamine hydrochloride was obtained through methylation,Dakin-West reaction,condensation with methylamine and salification starting from 2-hydroxyphenylacetic acid,the effects of catalyst,the ratio of materials and the solvent of recrystallization on the yields were discussed.The optimal molar ratio of 2-hydroxyphenylacetic acid,methyl sulfate,sodium hydroxide,acid anhydride,N-methylimidazole was 1:2.5:4.0:2.5:0.2 in the intermediate preparation of 2-methoxyphenylacetone,the optimal mass ratio of 2-methoxyphenylacetone,33% methylamine in ethanol and Pt/C was 1:0.6:0.01 in the preparation of methoxyphenamine,the optimal mass ratio of toluene and ethanol was 5:1 in recrystallization,the total yield was 46.5%(calculated from 2-hydroxyphenylacetic acid).The process has industrialization prospect.
出处
《化工生产与技术》
CAS
2012年第1期7-9,67,共3页
Chemical Production and Technology
