HRID1020053
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 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
- washwashed with water
- customThe organic layer was separated
- dry with materialdried over sodium sulfate
- concentrationconcentrated
- customThe obtained crude residue