HRID1836977

反应详情

EQUATION

反应方程式

HRID 1836977 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 2-(methylsulfonyl)-4-[4-(methylsulfonyl)phenyl]-6-(trifluoromethyl)pyrimidine (0.50 g, 1.31 mmol) in MeCN (10 ml) was added cyclohexylamine (0.50 ml) and the resultant solution heated under reflux for 26 h. The cooled reaction mixture was concentrated in vacuo and the residue partitioned between 2N HCl and ethyl acetate. The organic phase was separated, washed with 2N HCl then water and concentrated in vacuo to an off-white solid. This solid was crystalised from 5% AcOH/MeOH and dried in vacuo to give the title compound as a white solid (0.27 g, 52%).

WORKUP

后处理

  1. temperatureunder reflux for 26 h
  2. customThe cooled reaction mixture
  3. concentrationwas concentrated in vacuo
  4. customthe residue partitioned between 2N HCl and ethyl acetate
  5. customThe organic phase was separated
  6. washwashed with 2N HCl
  7. concentrationwater and concentrated in vacuo to an off-white solid
  8. customThis solid was crystalised from 5% AcOH/MeOH
  9. customdried in vacuo