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 (2-bromopyridin-3-yl)methanol (100 mg) in tetrahydrofuran (1 ml), 36 mg of dichloro(1,1′-bis(diphenylphosphino)ferrocene)nickel(II) and 0.8 ml of isobutyl magnesium bromide (2.0M diethyl ether solution) were added under ice-cooling, and the reaction solution was stirred at the same temperature for 4 hours. To the reaction solution was added saturated aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate. The combined organic layers were washed with a saturated saline solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the residue obtained was purified by silica gel column chromatography (eluent: hexane/ethyl acetate (98:2-50:50)) to afford the title compound as a yellow oil.
WORKUP
后处理
- temperaturecooling
- extractionthe mixture was extracted with ethyl acetate
- washThe combined organic layers were washed with a saturated saline solution
- dry with materialdried over anhydrous sodium sulfate
- distillationThe solvent was distilled off under reduced pressure
- customthe residue obtained
- customwas purified by silica gel column chromatography (eluent: hexane/ethyl acetate (98:2-50:50))