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
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
To a solution of 2-phenoxynicotinic acid (2.0 g) in tetrahydrofuran (20 ml), 9.5 ml of borane-tetrahydrofuran complex (1.17M tetrahydrofuran solution) was added, and the reaction solution was stirred overnight at 50° C. The reaction solution was cooled, 14 ml of 1N aqueous sodium hydroxide was added under ice-cooling, and the reaction solution was stirred for 1 hour. The reaction solution was diluted with saturated aqueous ammonium solution, extracted with diethyl ether, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue obtained was purified by silica gel column chromatography (eluent: ethyl acetate/hexane (0:100-50:50)) to afford the title compound as a colorless oil.
WORKUP
后处理
- temperatureThe reaction solution was cooled
- temperaturecooling
- stirringthe reaction solution was stirred for 1 hour
- extractionextracted with diethyl ether
- dry with materialdried over anhydrous magnesium sulfate
- distillationThe solvent was distilled off under reduced pressure
- customthe residue obtained
- customwas purified by silica gel column chromatography (eluent: ethyl acetate/hexane (0:100-50:50))