HRID1771638
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
- 60 °C
PROCEDURE
实验过程
To a solution of 2-fluoro-5-(3-fluorophenyl)-N-(3-hydroxy-2,6-dimethyl-phenyl)benzamide (400 mg, 1.13 mmol, 1.0 eq) in THF under N2 was added dropwise a solution of BH3 (5.65 mL, 1M in THF, 5.65 mmol, 5.0 eq). The reaction mixture was heated to 60° C. and stirred under N2 for 3 h. After cooling, the resulting mixture was quenched by addition of 1 M HCl and water and the aqueous layer extracted with EtOAc. The organic extract was dried (Na2SO4), filtered, evaporated in vacuo and purified by column chromatography (EtOAc:petroleum ether, 0:1 to 1:4) to give the title product as yellow oil (340 mg, 89%).
WORKUP
后处理
- temperatureAfter cooling
- customthe resulting mixture was quenched by addition of 1 M HCl and water
- extractionthe aqueous layer extracted with EtOAc
- extractionThe organic extract
- dry with materialwas dried (Na2SO4)
- filtrationfiltered
- customevaporated in vacuo
- custompurified by column chromatography (EtOAc:petroleum ether, 0:1 to 1:4)