水相合成S-正辛基-5,5-二苯基-2-硫代海因的绿色工艺

摘要

S-n-octyl-5,5-diphenyl-2-thiohydantoin was synthesized using 5,5-diphenyl-2-thiohydantoin and n-octyl bromide as the raw materials by phase transfer catalysis in alkali solution.The effects of the amounts of n-octyl bromide and alkali,phase transfer agents and their dosages,and reaction time on the yield were investigated.The results showed that the yield of S-n-octyl-5,5-diphenyl-2-thiohydantoin with high purity was 85％ under the optimal condition was as follows:5,5-diphenyl-2-thiohydantoin 50 mmol,n-octyl bromide 55 mmol,KOH 50 mmol,octadeca tertiary amine 0.2 g,H2O 50 mL,and reflux time 4 h.The product was characterized by IR,1H NMR,13C NMR and MS.%以5,5-二苯基-2-硫代海因和溴代正辛烷为原料,在碱水溶液中相转移催化合成S-正辛基-5,5-二苯基-2-硫代海因,考察溴代正辛烷用量、氢氧化钾用量、相转移剂种类和用量以及反应时间对产率的影响.确定较佳工艺条件为:5,5-二苯基-2-硫代海因50 mmol,溴代正辛烷55 mmol,氢氧化钾50 mmol,十八叔胺0.2g,水50 mL,回流反应4h,可得到高纯度S-正辛基-5,5-二苯基-2-硫代海因,产率达85％.产品结构经IR、1H NMR、13C NMR及MS进行了表征.