HRID1836977
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
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
- temperatureunder reflux for 26 h
- customThe cooled reaction mixture
- concentrationwas concentrated in vacuo
- customthe residue partitioned between 2N HCl and ethyl acetate
- customThe organic phase was separated
- washwashed with 2N HCl
- concentrationwater and concentrated in vacuo to an off-white solid
- customThis solid was crystalised from 5% AcOH/MeOH
- customdried in vacuo