3-Fluoro-4-nitrophenol → 4-Amino-3-fluorophenol
反応式
[F:1][C:2]1[CH:3]=[C:4]([OH:11])[CH:5]=[CH:6][C:7]=1[N+:8]([O-])=O.C(O[K])=O>C1COCC1.O.[Pd]>[NH2:8][C:7]1[CH:6]=[CH:5][C:4]([OH:11])=[CH:3][C:2]=1[F:1]参加物
5
反応条件
- 温度
- 50 °C
実験手順
A suspension of 3-fluoro-4-nitrophenol (2.0 g, 12.73 mmol), 10% Pd/C (0.4 g) and HCOOK (8.75 g, 101.85 mmol) in THF/H2O (70 mL/20 mL) was stirred at 50° C. for 5 hours, then cooled to rt, and filtered through CELITE®. The filtrate was diluted with water (30 mL) and extracted with THF (50 mL). The organic layer was dried over Na2SO4 and concentrated in vacuo. The residue was diluted with water (50 mL) and extracted with DCM (50 mL). The organic layer was dried over anhydrous Na2SO4 and concentrated in vacuo to give the title compound as a brown solid (1.17 g, 72.3%).
後処理
- temperaturecooled to rt
- filtrationfiltered through CELITE®
- additionThe filtrate was diluted with water (30 mL)
- extractionextracted with THF (50 mL)
- dry with materialThe organic layer was dried over Na2SO4
- concentrationconcentrated in vacuo
- additionThe residue was diluted with water (50 mL)
- extractionextracted with DCM (50 mL)
- dry with materialThe organic layer was dried over anhydrous Na2SO4
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-ce6b1edf87cc4a6695d4e06fe3070df3
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09326975B2
反応ノート
読み込み中…