HRID1868378

反应详情

EQUATION

反应方程式

HRID 1868378 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-chloro-4-trifluoromethyl-pyrimidin-5-carbonyl chloride (750 mg, ex Maybridge) in dichloromethane (15 ml) at −400 was added dropwise over 30 minutes a solution of cyclohexanemethanamine (0.35 ml, ex Lancaster) and triethylamine (0.41 ml) in dichloromethane (15 ml). Dichloromethane was removed under reduced pressure and ethyl acetate (20 ml) added. The solution was washed sequentially with water, 5% sodium bicarbonate solution and water, dried (MgSO4), evaporated and triturated with ether:hexane to afford 2-chloro-trifluoromethyl-pyrimidine-5-carboxylic acid cyclohexylmethyl-amide (666 mg).

WORKUP

后处理

  1. customDichloromethane was removed under reduced pressure and ethyl acetate (20 ml)
  2. additionadded
  3. washThe solution was washed sequentially with water, 5% sodium bicarbonate solution and water
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. customtriturated with ether