HRID746243
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
Ethylene bromohydrin (5.4 g) was added dropwise to a mixture of 1-(3-chlorophenyl)piperazine hydrochloride (5 g), potassium carbonate powder (12 g) and N,N-dimethylformamide (35 ml) with stirring. The mixture was further stirred at room temperature overnight, then diluted with 100 ml of water and extracted with ethyl ether. The ethyl ether layer was washed with saturated aqueous sodium chloride and dried over Na2SO4. The solvent was distilled off and the residue was purified by silica gel chromatography [eluent: ethyl acetate-methanol (4:1)] to give 4.06 g (78.6%) of 4-(3-chlorophenyl)-1-piperazineethanol as an oil.
WORKUP
后处理
- stirringThe mixture was further stirred at room temperature overnight
- extractionextracted with ethyl ether
- washThe ethyl ether layer was washed with saturated aqueous sodium chloride
- dry with materialdried over Na2SO4
- distillationThe solvent was distilled off
- customthe residue was purified by silica gel chromatography [eluent: ethyl acetate-methanol (4:1)]