HRID451399
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
A solution of 2-bromo-6-phenyl-cyclohexanone (4.32 g, 17 mmol) and thiourea (1.18 g, 16 mmol) in EtOH (150 mL) was heated to reflux for 12 hours. The solvent was evaporated, diethyl ether was added to the residue and stirred at room temperature for 1 hour, the solid filtered off and washed with diethylether. The solid was dissolved in ethyl acetate and the organic phase was washed three times with sodium carbonate solution. The organic phase was dried over sodium sulfate, the solvent was evaporated to give the title compound as a white solid (3.46 g, 88%). MS ISP (m/e): 231.1 [(M+H)+].
WORKUP
后处理
- temperatureto reflux for 12 hours
- customThe solvent was evaporated
- additiondiethyl ether was added to the residue
- filtrationthe solid filtered off
- washwashed with diethylether
- dissolutionThe solid was dissolved in ethyl acetate
- washthe organic phase was washed three times with sodium carbonate solution
- dry with materialThe organic phase was dried over sodium sulfate
- customthe solvent was evaporated