Acetic Acid → 4-(Difluoromethoxy)-3-methylaniline
反応式
[F:1][CH:2]([F:14])[O:3][C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-])=O)=[CH:6][C:5]=1[CH3:13].C(O)(=O)C>C(O)C.O.[Fe]>[NH2:10][C:7]1[CH:8]=[CH:9][C:4]([O:3][CH:2]([F:1])[F:14])=[C:5]([CH3:13])[CH:6]=1参加物
6
実験手順
To a solution of 1-(difluoromethoxy)-2-methyl-4-nitrobenzene (10 g, 48.28 mmol) in ethanol (150 mL) and water (150 mL) was added iron powder (12 g, 214.29 mmol). Acetic acid (cat. amount) was added dropwise with stirring and the reaction mixture was heated at reflux for 20 minutes. The mixture was cooled to room temperature and solids were removed by filtration. Volatiles were removed in vacuo and the aqueous solution was extracted with EtOAc (3×150 mL). The combined organic layers were dried over Na2SO4 and concentrated in vacuo to provide 8 g (95%) of 4-amino-1-difluoromethoxy-2-methyl-benzene.
後処理
- temperaturethe reaction mixture was heated
- temperatureat reflux for 20 minutes
- customsolids were removed by filtration
- customVolatiles were removed in vacuo
- extractionthe aqueous solution was extracted with EtOAc (3×150 mL)
- dry with materialThe combined organic layers were dried over Na2SO4
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-267cecc992f84a0db18c5e58c551105a
- 出典データセット
- uspto-grants-2009_02
- 特許番号
- US07494999B2
反応ノート
読み込み中…