N,N-二(2-羟乙基)对甲苯磺酰胺与氯化亚砜的反应

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N,N-二(2-羟乙基)对甲苯磺酰胺(1)与SOCl_2反应,通常得化合物2. 文献报道采用过量SOCl_2作溶剂在130~140℃进行反应,但后处理较麻烦,且SOCl_2用量也较大.我们改用二甲苯作溶剂,并减少SOCl_2的用量及采用分次加入的方法,收到了较好的效果.在此反应过程中,意外地获得了一无色针状结晶,根据IR,~1H NMR,MS及元素分析证明此化合物为3.上述反应如控制反应条件可使1全部转化得3. The reaction of N, N-bis (2-hydroxyethyl) p-toluenesulfonamide (1) with SOCl 2 usually gives compound 2. It has been reported in the literature that excess SOCl 2 is used as the solvent at 130 to 140 ° C., but the post- SOCl_2 dosage is also larger.We use xylene as a solvent, and reduce the amount of SOCl_2 and the use of sub-added method, received good results.In this reaction, unexpectedly obtained a colorless needle-shaped crystals According to IR, ~ 1H NMR, MS and elemental analysis, this compound was proved to be 3. The above reaction can be converted to 3 if the reaction conditions are controlled.
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