4-Chloro-2-acetamidobenzoic acid → 2-Amino-4-chlorobenzoic acid
反応式
C([NH:4][C:5]1[C:6](=[CH:10][CH:11]=[C:12]([Cl:14])[CH:13]=1)[C:7]([OH:9])=[O:8])(=O)C>Cl>[Cl:14][C:12]1[CH:13]=[C:5]([NH2:4])[C:6](=[CH:10][CH:11]=1)[C:7]([OH:9])=[O:8]参加物
3
反応条件
- 温度
- 80 °C
実験手順
The damp N-acetyl-4-chloroanthranilic acid is suspended in 400 ml of concentrated hydrochloric acid (12M) and stirred and heated at 80° C. for 8 hours. The mixture is cooled to 10° C. and the resulting 4-chloroanthranilic acid hydrochloride is recovered by filtration. The solid is suspended in 300 ml water and sodium acetate is added, portionwise until the pH is 5. The resulting 4-chloroanthranilic acid is recovered by filtration and recrystallized from the minimum of hot ethanol. The final yield of off-white crystals was about 50 g, melting at about 239°-240° C.
後処理
- temperatureThe mixture is cooled to 10° C.
- filtrationthe resulting 4-chloroanthranilic acid hydrochloride is recovered by filtration
- additionsodium acetate is added, portionwise until the pH is 5
- filtrationThe resulting 4-chloroanthranilic acid is recovered by filtration
- customrecrystallized from the minimum of hot ethanol
出典と根拠
- ORDレコード
- ord-50e9b283033b4c4dabaa4c15d1720d64
- 出典データセット
- uspto-grants-1994_11
- 特許番号
- US05364767
反応ノート
読み込み中…