N-(2,6-Difluoro-3-hydroxy-phenyl)-5-(3,4-difluorophenyl)-2,3-dimethyl-benzamide → HCID 89444144、化合物
反応式
[F:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[C:4]([F:9])[C:3]=1[NH:10][C:11](=O)[C:12]1[CH:17]=[C:16]([C:18]2[CH:23]=[CH:22][C:21]([F:24])=[C:20]([F:25])[CH:19]=2)[CH:15]=[C:14]([CH3:26])[C:13]=1[CH3:27]>C1COCC1>[F:25][C:20]1[CH:19]=[C:18]([C:16]2[CH:15]=[C:14]([CH3:26])[C:13]([CH3:27])=[C:12]([CH2:11][NH:10][C:3]3[C:2]([F:1])=[C:7]([OH:8])[CH:6]=[CH:5][C:4]=3[F:9])[CH:17]=2)[CH:23]=[CH:22][C:21]=1[F:24]参加物
3
反応条件
- 温度
- 60 °C
実験手順
To a solution of N-(2,6-difluoro-3-hydroxy-phenyl)-5-(3,4-difluorophenyl)-2,3-dimethyl-benzamide (90 mg, 0.23 mmol, 1.0 eq) in THF (1.5 mL) under N2 was added dropwise a solution of BH3 (1M in THF, 1.03 mL, 1.03 mmol, 4.6 eq) at 0° C. The reaction mixture was heated at 60° C. overnight then cooled and the reaction quenched with water. The aqueous layer was extracted with EtOAc and the combined organic extracts were washed with brine, dried (Na2SO4), filtered and evaporated in vacuo. The residue obtained was purified by column chromatography (petroleum ether:EtOAc, 30:1 to 15:1) to give the title compound as a colorless oil (70 mg, 81%).