Acetic Anhydride → 4-Methylthio-2-acetoxybenzoic acid
反応式
[CH3:1][S:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[C:5]([OH:12])[CH:4]=1.[C:13](OC(=O)C)(=[O:15])[CH3:14]>S(=O)(=O)(O)O.O>[CH3:1][S:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[C:5]([O:12][C:13](=[O:15])[CH3:14])[CH:4]=1参加物
5
反応条件
- 温度
- 75 °C
実験手順
To a mixture of 4-methylthio-2-hydroxybenzoic acid (50.0 g, 272 mmol) and acetic anhydride (77.0 mL, 815 mmol) was added 36 N sulfuric acid (0.45 mL, 8.16 mmol) and the mixture was heated to 75° C. for 1 h. To the reaction mixture was added H2O (200 mL), and it was stirred for 18 h. A white precipitate was collected, triturated with dichloromethane, (100 mL), diluted with 20% Et2O/hexanes (300 mL), and filtered to give the title compound as a white solid (49 g, 80%).
後処理
- customA white precipitate was collected
- customtriturated with dichloromethane, (100 mL)
- additiondiluted with 20% Et2O/hexanes (300 mL)
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-5183a123dbf14c009a3cb75d15b065d2
- 出典データセット
- uspto-grants-2009_11
- 特許番号
- US07615568B2
反応ノート
読み込み中…