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
Under nitrogen atmosphere, over a suspension of 0.55 g (13.72 mmol) of sodium hydride 60% in paraffin oil in 10 ml of DMF, a solution of 2.5 g (9.1 mmol) of 4-(1H-pyrrolo[2,3-b]pyridin-3-yl)-piperidine-1-carboxylic acid ethyl ester in 10 ml of DMF was added. After 30 minutes, a solution of 1.2 ml of 4-bromobutane in 2 ml of DMF was added. The crude mixture was stirred at room temperature for 15 hours. The solvent was removed under reduced pressure and the crude was partionated between ethyl acetate and water. The organic phase was dried over sodium sulphate, filtered and the solvent was removed under reduced pressure affording 3.1 g of 4-(1-butyl-1H-pyrrolo[2,3-b]pyridin-3-yl)-piperidine-1-carboxylic acid ethyl ester.
WORKUP
后处理
- customThe solvent was removed under reduced pressure
- dry with materialThe organic phase was dried over sodium sulphate
- filtrationfiltered
- customthe solvent was removed under reduced pressure