N,N-二甲氨基磺酰氯合成工艺的优化

Improvent for preparation technology of dimethylsulfamoyl chloride

以磺酰氯和二甲胺盐酸盐为原料在三乙胺催化剂的作用下合成N,N-二甲氨基磺酰氯,并进行了单因素实验,在此基础上运用响应面法对N,N-二甲氨基磺酰氯合成工艺进行了优化,优化调整后的工艺条件为:反应温度9℃,二氯乙烷用量250 mL,n(二甲胺盐酸盐)∶n(磺酰氯)=1.0∶1.2。在该工艺条件下重复实验,N,N-二甲氨基磺酰氯平均收率为77.5%,与模型预测收率相符。

Using sulfuryl chloride and dimethylamine hydrochloride as raw materials,triethylamine as acid binding agent dimethylsulfamoyl chloride was synthesized,and the synthesis process had been optimized by the single factor and response surface method.The optimized process conditions were as followings:reaction temperature was 9℃,dichloroethane dosage was 250 mL,n(dimethylamine hydrochloride)∶n(sulfuryl chloride)=1.0∶1.2.The average yield of dimethylsulfamoyl chloride was of 77.5%,and it was consistent with the prediction model.