2-aminosulfonyl-6-isopropyl-N,N-diethylbenzamide → 4-Isopropylsaccharin
反応式
N[S:2]([C:5]1[CH:17]=[CH:16][CH:15]=[C:14]([CH:18]([CH3:20])[CH3:19])[C:6]=1[C:7]([N:9](CC)CC)=[O:8])(=[O:4])=[O:3]>C(O)(=O)C>[CH:18]([C:14]1[CH:15]=[CH:16][CH:17]=[C:5]2[C:6]=1[C:7](=[O:8])[NH:9][S:2]2(=[O:4])=[O:3])([CH3:20])[CH3:19]参加物
3
実験手順
A solution of 2-aminosulfonyl-6-isopropyl-N,N-diethylbenzamide (60 g) in acetic acid (400 mL) was refluxed for 24 hours, then cooled to room temperature. The solvent was removed under vacuum. The oily residue was dissolved in water (500 mL) and the pH was adjusted to 1 with hydrochloric acid (2N). The crude product was collected by filtration, washed with water (300 mL), dried at 60° C. under vacuum for 18 hours and recrystallized from ether-hexane to give 4-isopropylsaccharin (40 g, 90% yield, m.p. 177° C.).
後処理
- customThe solvent was removed under vacuum
- dissolutionThe oily residue was dissolved in water (500 mL)
- filtrationThe crude product was collected by filtration
- washwashed with water (300 mL)
- customdried at 60° C. under vacuum for 18 hours
- customrecrystallized from ether-hexane
出典と根拠
- ORDレコード
- ord-bdc8ff4f39b6452db6ac7a28a047d567
- 出典データセット
- uspto-grants-1995_11
- 特許番号
- US05466701
反応ノート
読み込み中…