反应详情

温度

60 °C

To a solution of N-(2,6-difluoro-3-hydroxy-phenyl)-2-fluoro-3-(3-fluorophenyl)-5-methoxy-benzamide (300 mg, 0.77 mmol, 1.0 eq) in THF (10 mL) at 0° C. under N2 was added a solution of BH3 (1M in THF, 4 mL, 4.0 mmol, 5.2 eq) dropwise. The reaction mixture was heated to 60° C. and stirred for 1.5 h. The reaction was cooled to room temperature then quenched by addition of 1M HCl. The mixture was stirred at room temperature for 1.5 h, then extracted with EtOAc. The organic extract was washed with water and brine, dried (Na2SO4), filtered and evaporated in vacuo. The residue was purified by column chromatography (EtOAc:petroleum ether, 0:1 to 1:4) to give the title compound as a yellow oil (180 mg, 62%).

1. temperatureThe reaction was cooled to room temperature
2. customthen quenched by addition of 1M HCl
3. stirringThe mixture was stirred at room temperature for 1.5 h
4. extractionextracted with EtOAc
5. extractionThe organic extract
6. washwas washed with water and brine
7. dry with materialdried (Na2SO4)
8. filtrationfiltered
9. customevaporated in vacuo
10. customThe residue was purified by column chromatography (EtOAc:petroleum ether, 0:1 to 1:4)