HRID451399

反应详情

EQUATION

反应方程式

HRID 451399 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureto reflux for 12 hours
  2. customThe solvent was evaporated
  3. additiondiethyl ether was added to the residue
  4. filtrationthe solid filtered off
  5. washwashed with diethylether
  6. dissolutionThe solid was dissolved in ethyl acetate
  7. washthe organic phase was washed three times with sodium carbonate solution
  8. dry with materialThe organic phase was dried over sodium sulfate
  9. customthe solvent was evaporated