HRID1020053

反应详情

EQUATION

反应方程式

HRID 1020053 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 6-(2-methoxy-phenyl)-pyrimidin-4-ylamine (XXIV) (5 g) in 20 ml of dichloromethane was added 4-dimethylaminopyridine (1.2 eq) followed by dropwise addition of 3-chlorocarbonyl-piperidine-1-carboxylic acid benzyl ester (XXV) (1.1 eq.) at room temperature. The reaction mixture was stirred for 2 hours and then washed with water. The organic layer was separated, dried over sodium sulfate and concentrated. The obtained crude residue was passed through a pad of silica gel eluting with 25% ethyl acetate in hexane to provide 3-[6-(2-methoxy-phenyl)-pyrimidin-4-ylcarbamoyl]-piperidine-1-carboxylic acid benzyl ester (XXVI) (5.1 g).

WORKUP

后处理

  1. washwashed with water
  2. customThe organic layer was separated
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated
  5. customThe obtained crude residue