Water → 1-Chloro-7-trifluoromethyl-2-aminonaphthalene
反応式
[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([C:12]([F:15])([F:14])[F:13])[CH:10]=2)[CH:5]=[CH:4][C:3]=1[NH:16]C(=O)C.O.S(=O)(=O)(O)O>C(O)C>[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([C:12]([F:14])([F:15])[F:13])[CH:10]=2)[CH:5]=[CH:4][C:3]=1[NH2:16]参加物
5
実験手順
A mixture of 1-chloro-7-trifluoromethyl-2-acetamidonaphthalene (700 mg, 2.43 mmol), water (3 mL) and concentrated sulfuric acid (3 mL in ethanol (6 mL) is heated to reflux temperature under a N2 atmosphere for 1 hour. After cooling to room temperature, the mixture is extracted with EtOAc. The extracts are washed with water, brine, dried (Na2SO4) and concentrated. Flash chromatography on silica gel (3:1 hexanes/EtOAc) gives 1-chloro-7-trifluoromethyl-2-aminonaphthalene as a white solid.
後処理
- temperatureis heated
- temperatureto reflux temperature under a N2 atmosphere for 1 hour
- extractionthe mixture is extracted with EtOAc
- washThe extracts are washed with water, brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-391daaa983604245b8dadcbb8a961258
- 出典データセット
- uspto-grants-2007_04
- 特許番号
- US07202364B2
反応ノート
読み込み中…