水相合成S-正辛基-5,5-二苯基-2-硫代海因的绿色工艺

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0.2 g,水50 mL,回流反应4 h,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。

A green procedure for water phase synthesis of S-n-octyl-5,5-diphenyl-2-thiohydantoin

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 noctyl 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.