HRID1771835
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 N-(2,6-difluoro-3-hydroxy-phenyl)-2,3-dimethyl-5-phenyl-benzamide (210 mg, 0.6 mmol, 1.0 eq) in THF (4 mL) at 0° C. was added dropwise a solution of BH3 (1M in THF, 3.6 mL, 3.6 mmol, 6.0 eq). The reaction mixture was heated at 60° C. for 5 h, then cooled and quenched by addition of water. The aqueous layer was extracted with EtOAc and the combined organic extracts were washed with water and brine, dried (Na2SO4), filtered and evaporated in vacuo. The residue obtained was purified by column chromatography (petroleum ether:EtOAc, 100:0 to 10:1) to give the title compound as colorless oil (120 mg, 60%).
WORKUP
后处理
- temperaturecooled
- customquenched by addition of water
- extractionThe aqueous layer was extracted with EtOAc
- washthe combined organic extracts were washed with water and brine
- dry with materialdried (Na2SO4)
- filtrationfiltered
- customevaporated in vacuo
- customThe residue obtained
- customwas purified by column chromatography (petroleum ether:EtOAc, 100:0 to 10:1)