HRID1087113
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
5.0 g of 4-[3-(ethylamino)-2-hydroxypropoxy]-benzonitrile and 4.0 g of 1-chloro-3-(phenylthio) propane was dissolved in 70 ml of acetonitrile and mixed with 6.4 g potassium carbonate and 8.0 g of sodium iodide. The mixture was refluxed over night, filtrated, evaporated and the residue was dissolved in 2 M hydrochloric acid. This acidic waterlayer was washed with two portions of diethylether, alkalized with 10 M sodium hydroxide and extracted with three portions of dichlorometane. The combined layers of dichloromethane were dried over sodium sulphate and evaporated. The oily residue was purified by column chromatography on silica gel. Yield: 2.1 g of the title compound.
WORKUP
后处理
- temperatureThe mixture was refluxed over night
- filtrationfiltrated
- customevaporated
- dissolutionthe residue was dissolved in 2 M hydrochloric acid
- washThis acidic waterlayer was washed with two portions of diethylether
- extractionextracted with three portions of dichlorometane
- dry with materialThe combined layers of dichloromethane were dried over sodium sulphate
- customevaporated
- customThe oily residue was purified by column chromatography on silica gel