| N,N-二甲基乙酰胺二甲基缩醛的合成工艺优化 |
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| 引用本文： | 张创军,徐茂梁,张倩,王歌扬.N,N-二甲基乙酰胺二甲基缩醛的合成工艺优化[J].应用化工,2011,40(8):1393-1394. |
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| 作者姓名： | 张创军 徐茂梁 张倩 王歌扬 |
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| 作者单位： | 西安近代化学研究所,陕西 西安,710065 |
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| 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1 h,反应时间为1.5 h。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%)。
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| 关 键 词： | DMACA 甲醇钠 硫酸二甲酯 亚胺络合物 合成工艺 |
Optimization for the synthesis of DMACA |
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| ZHANG Chuang-jun,XU Mao-liang,ZHANG Qian,WANG Ge-yang.Optimization for the synthesis of DMACA[J].Applied chemical industry,2011,40(8):1393-1394. |
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| Authors: | ZHANG Chuang-jun XU Mao-liang ZHANG Qian WANG Ge-yang |
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| Affiliation: | ZHANG Chuang-jun,XU Mao-liang,ZHANG Qian,WANG Ge-yang(Xi'an Modern Chemistry Research Institute,Xi'an 710065,China) |
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| Abstract: | An optimized synthesis process of DMACA(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 ℃,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%. |
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| Keywords: | DMACA sodium methoxide dimethyl sulfate imine complex synthesis process |
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