4-Chloro-3-methylphenol → 4-Chloro-3-methylphenyl acetate
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][C:3]=1[CH3:9].[C:10](OC(=O)C)(=[O:12])[CH3:11]>S(=O)(=O)(O)O.O>[C:10]([O:8][C:5]1[CH:6]=[CH:7][C:2]([Cl:1])=[C:3]([CH3:9])[CH:4]=1)(=[O:12])[CH3:11]参加物
5
実験手順
43.0 g (0.30 mol) of 4-chloro-3-methylphenol, 34 ml (0.36 mol) of acetic anhydride and a few drops of concentrated sulfuric acid were stirred for 2 h at 60° C. in a 250 ml flask equipped with a reflux condenser. The reaction mixture was cooled to room temperature, poured into 200 ml of water and stirred for 1 h at room temperature. The mixture was then extracted with 400 ml of diethyl ether. The organic phase was dried over magnesium sulfate and the ether was distilled off. The raw product is subsequently distilled under reduced pressure (b.p. 65-68° C., 20 mbar).
後処理
- customequipped with a reflux condenser
- extractionThe mixture was then extracted with 400 ml of diethyl ether
- dry with materialThe organic phase was dried over magnesium sulfate
- distillationthe ether was distilled off
- distillationThe raw product is subsequently distilled under reduced pressure (b.p. 65-68° C., 20 mbar)
出典と根拠
- ORDレコード
- ord-2abe76b980254f9eb3d2fd29f5a44d81
- 出典データセット
- uspto-grants-2004_03
- 特許番号
- US06699405B2
反応ノート
読み込み中…