阿比朵尔合成曼尼希反应工艺研究

摘要

Using 6-bromo-5-hydroxy-1-methyl-2-phenyl methyl sulfide indole-3-carboxylic acid ethyl ester as raw material,the Mannich reaction of arbidol hydrochloride.The optimum synthesis process parameters were as follows∶ n(6-bromo-5-hydroxy-l-methyl-2-phenyl methyl sulfide indole-3-carboxylic acid ethyl ester) ∶ n (dimethylamine) =1 ∶ 3,n (dimethylamine) ∶ n (methanal) =2.2∶ 1,reaction time 2 h,reaction temperature 65 ℃.Under this condition,the yield was over 83％,the purity was more than 99.0％.%采用6-溴-5-羟基-1-甲基-2-苯硫甲基吲哚-3-羧酸乙酯为原料,经曼尼希反应合成盐酸阿比朵尔.最佳合成工艺参数为:n(6-溴-5-羟基-1-甲基-2-苯硫甲基吲哚-3-羧酸乙酯)∶n(二甲胺)=1∶3,n(二甲胺):n(甲醛)=2.2∶1,反应时间2h,反应温度65℃.在此条件下,收率为83％以上,纯度为99.0％以上.