摘要
目的 探索有机药物中间体乙烷磺酰氯的最佳合成方法。方法 通过探讨对比乙烷磺酰氯几种合成方法的收率、成本、产业化存在的问题 ,初步确定乙硫醇氯化法具有更好的推广价值 ,并对该方法的工艺条件进行优化。结果 乙硫醇氯化合成乙烷磺酰氯的优惠实验条件 :向配比为n(C2 H5SH)∶n(H2 O) =1∶3～ 4的料液中加入相转移催化剂 ,搅拌下通入氯气n(C2 H5SH)∶n(Cl2 ) =1∶3.14 ,分段采用较低的氯化温度 ,氯化温度前期不超过 5℃ ,中后期不超过 2 0℃ ,反应完毕分层 ,下部油相w(乙烷磺酰氯 )≥ 95 % ,以乙硫醇计收率≥ 95 %。以无水氯化钙干燥 ,真空蒸馏得w(乙烷磺酰氯 )≥ 98%。结论 乙硫醇氯化合成乙烷磺酰氯以其产品收率高 ,质量好 ,成本低 ,原料易得 ,操作简便等优点被认为是一条最佳合成方法。
Objective: To investigate the optimal method of synthesizing the organic medical intermediate ethanesulfonyl chloride. Methods: The yield, cost and industrial problems of several methods for preparing ethanesulfonyl chloride were discussed and compared. Chlorination of ethyl mercaptan was primarily determined to be valuable in industry. The processing conditions were optimized here. Results: The optimized processing conditions were decided: 1 mol ethyl mercapan, 3～4 mol water and phase transfer catalyst were added to a stirring reactor. 3.14 mol chorine was blown to the bottom of reactor, controling the reacting temperature below 5℃ in the prime period and below 20 ℃ in the middle and later period. After the reation ended, the bottom oil phase was separated, determined by GC, content of ethanesulfonyl choride 95%, yield 95% base on ethyl mercaptan. Dried with CaCl2, distilled under vacuum, ethanesulfonyl chloride piurty 98% was obtained. Conclusion: Of all these methods, chlorination of ethyl mercaptan is the most reliable process for its good yield, high purity, low cost and easy operation.
出处
《泰山医学院学报》
CAS
2004年第4期270-272,共3页
Journal of Taishan Medical College
关键词
乙烷磺酰氯
乙基磺酰氯
乙硫醇
ethanesulfonyl chloride
ethylsulfonyl chloride
ethyl mercaptan
