HRID2108132
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Phenethylmercaptan (2.0 g) and potassium hydroxide (0.81 g) in methanol (15 ml) were stirred together under nitrogen for 15 min. 2-Chloroethanol (2.33 g) was added and the solution stirred under nitrogen for 6 h. 2N hydrochloric acid was added to acidify the mixture to pH5, and the methanol evaporated in vacuo. The residue was partitioned between water (100 ml) and diethyl ether (100 ml) and separated. The aqueous phase was re-extracted with diethyl ether (100 ml) and the combined ethereal layers dried and evaporated in vacuo to give an oil. Purification by FCC eluting with System F (3:1) gave the title compound (1.80 g) as a colourless oil. T.l.c. (diethyl ether) Rf 0.70
WORKUP
后处理
- customthe methanol evaporated in vacuo
- customThe residue was partitioned between water (100 ml) and diethyl ether (100 ml)
- customseparated
- extractionThe aqueous phase was re-extracted with diethyl ether (100 ml)
- customthe combined ethereal layers dried
- customevaporated in vacuo
- customto give an oil
- customPurification by FCC
- washeluting with System F (3:1)