Acetic Anhydride → 1,3-Difluoro-5-(2-nitroethenyl)benzene
反応式
C(OC(=O)C)(=O)C.[F:8][C:9]1[CH:10]=[C:11]([CH:16](O)[CH2:17][N+:18]([O-:20])=[O:19])[CH:12]=[C:13]([F:15])[CH:14]=1>CN(C)C1C=CN=CC=1.ClCCl>[F:8][C:9]1[CH:10]=[C:11]([CH:16]=[CH:17][N+:18]([O-:20])=[O:19])[CH:12]=[C:13]([F:15])[CH:14]=1参加物
5
実験手順
Add acetic anhydride (160 mL) to a solution of 1-(3,5-difluorophenyl)-2-nitroethanol (330 g) and 4-dimethylaminopyridine (18 g) in dichloromethane (1000 mL), over 30 minutes and stir the reaction mixture overnight. Dilute with dichloromethane (600 mL) and wash with 2% aqueous hydrochloric acid, saturated aqueous sodium chloride, saturated aqueous sodium bicarbonate, dry (magnesium sulfate) and concentrate. Wash the crude with hexanes to give the desired compound (220 g).
後処理
- washwash with 2% aqueous hydrochloric acid, saturated aqueous sodium chloride, saturated aqueous sodium bicarbonate
- dry with materialdry (magnesium sulfate)
- concentrationconcentrate
- washWash the crude with hexanes
出典と根拠
- ORDレコード
- ord-1080cca5ae27486f9ef3c8ea4c9fcc42
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07745438B2
反応ノート
読み込み中…