Hydrochloric Acid → 2-Acetoxy-5-bromo-6-methylbenzoic acid
反応式
[OH:1][C:2]1[CH:10]=[CH:9][C:8]([Br:11])=[C:7]([CH3:12])[C:3]=1[C:4]([OH:6])=[O:5].[C:13](OC(=O)C)(=[O:15])[CH3:14].N1C=CC=CC=1.Cl>O.C(OCC)(=O)C>[C:13]([O:1][C:2]1[CH:10]=[CH:9][C:8]([Br:11])=[C:7]([CH3:12])[C:3]=1[C:4]([OH:6])=[O:5])(=[O:15])[CH3:14]参加物
7
実験手順
A mixture of 1B (6.93 g, 30 mmol), acetic anhydride (3.5 ml, 36 mmol) and pyridine (15 ml) is heated under reflux with stirring for 16 hours. The reaction mixture is diluted with water and ethyl acetate. The organic phase is acidified with dilute hydrochloric acid and washed with water twice. The organic phase is concentrated in vacuo and the residue is purified by flash chromatography (dichloromethane:methanol, 9:1 v/v) yielding the pure product as a yellow oil, 7.4 g, (90.3%).
後処理
- temperatureis heated
- temperatureunder reflux
- washwashed with water twice
- concentrationThe organic phase is concentrated in vacuo
- customthe residue is purified by flash chromatography (dichloromethane:methanol, 9:1 v/v)
出典と根拠
- ORDレコード
- ord-53b724b373e640f3b1a2566c1fdb3d86
- 出典データセット
- uspto-grants-2000_10
- 特許番号
- US06127570
反応ノート
読み込み中…