N,N-二甲基乙酰胺二甲基缩醛的合成工艺优化

摘要

报道了一种优化的N,N-二甲基乙酰胺二甲基缩醛(DMACA)合成工艺.该工艺使用液体甲醇钠,蒸除甲醇后悬浮在正己烷中,再和亚胺络合物反应.甲醇钠和硫酸二甲酯的摩尔比为1.2:1,-10℃滴加亚胺络合物,滴加时间为1h,反应时间为1.5h.本合成工艺产品收率高(由文献值25％～35％提高到75％～85％),纯度好( HPLC≥98％).%An optimized synthesis process of DM AC A (N,N-dimethyla-cetamide dimethyl acetal) was reported. The process used liquid sodium methoxide, liquid sodium methoxide reacted with imine complex after steamed away methanol and then suspended in hexane. The molar ratio of sodium methoxide to dimethyl sulfate was 1.2 :1, the reaction temperature was - 10 °C ,the dropping time was 1 h and the reaction time was 1.5 h. The yield was increased from 25% ~ 35% to 75% ~ 85% ,and the purity of the product was over 98%.