反应详情

温度

60 °C

To a solution of 2-fluoro-N-(6-fluoro-3-hydroxy-2-methyl-phenyl)-5-(3-fluorophenyl)-3-methyl-benzamide (404 mg, 1.1 mmol, 1.0 eq) in THF (10 mL) under N2 was added a solution of BH3 (1M in THF, 5.5 mL, 5.5 mmol, 5.0 eq) at room temperature. The reaction mixture was heated at 60° C. for 3 h, then cooled to room temperature and quenched with 1 M HCl. Water was added and the aqueous layer was extracted with EtOAc. The combined organic extracts were dried (Na2SO4), filtered and evaporated in vacuo. The crude residue obtained was purified by column chromatography (petroleum ether:EtOAc, 100:1 to 15:1) to give the title compound as a yellow oil (269 mg, 69%).

1. temperaturecooled to room temperature
2. customquenched with 1 M HCl
3. additionWater was added
4. extractionthe aqueous layer was extracted with EtOAc
5. dry with materialThe combined organic extracts were dried (Na2SO4)
6. filtrationfiltered
7. customevaporated in vacuo
8. customThe crude residue obtained
9. customwas purified by column chromatography (petroleum ether:EtOAc, 100:1 to 15:1)