Acetic Anhydride → 4-Acetamido-2-fluorobenzoic acid
反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([F:11])[CH:3]=1.[C:12](OC(=O)C)(=[O:14])[CH3:13]>C(O)(=O)C.O>[C:12]([NH:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([F:11])[CH:3]=1)(=[O:14])[CH3:13]参加物
5
反応条件
- 温度
- 60 °C
実験手順
A mixture of 4-amino-2-fluoro-benzoic acid (5.61 g, 36.2 mmol) and acetic anhydride (5.13 mL, 54.3 mmol) in 60 mL acetic acid was stirred at 60° C. overnight. The mixture was taken up in 250 mL water and stirred for 30 min. The precipitate was filtered and washed with water. The filtrate was washed with ethyl acetate. The organic phase was neutralized with sat. K2CO3 (aq) and concentrated i.vac. A small volume was left, the precipitate was filtered and combined with the first isolated precipitate.
後処理
- stirringstirred for 30 min
- filtrationThe precipitate was filtered
- washwashed with water
- washThe filtrate was washed with ethyl acetate
- concentrationconcentrated i.vac
- waitA small volume was left
- filtrationthe precipitate was filtered
出典と根拠
- ORDレコード
- ord-5cf10067f3d34ff3907db114aa523b5f
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08916599B2
反応ノート
読み込み中…