摘要
通过实验,分别对相转移催化剂法和DMF(二甲基甲酰胺)溶剂法合成新型促渗剂1,2-苯并异噻唑-3(2H)-2-丁基-1,1-二氧化物(噻酮)的工艺进行了研究.重点改进了原始DMF溶剂法的生产工艺,当温度为100℃,糖精钠、溴代正丁烷和DMF的物质的量的比为1∶1∶10时,产率超过88%.经减压精馏,溶剂DMF可回收循环使用,回收率达99%以上.实验中使用醇析法分离提纯产品,纯度(质量分数)达99%以上.改进的DMF溶剂法是一种更加经济、更适合工业化的合成工艺.
Two synthetic methods of 1,2-Benzisothiazol-3 (2 H)-one-2-butyl-1,1-dioxide (Thiazone, a novel skin penetration enhancer), such as the phase transfer catalysis method and DMF (N, N-dimethyllformamide) solvent method, were studied. Attention was paid to improving the DMF solution method. The yield of Thiazone was reached over 88 % by using the improved DMF solvent method at reaction temperature 100℃ and feed mole ratio 1 : 1 : 10 of sodium saccharin, butyl bromide and DMF. DMF could be reused by reduced pressure distillation and its recovery rate was over 99 %. The product could be purified well though ethanol extraction and its purity was over 99%. The improved DMF solvent method has advantages in economy and industrialization.
出处
《浙江大学学报(工学版)》
EI
CAS
CSCD
北大核心
2009年第3期468-471,共4页
Journal of Zhejiang University:Engineering Science