Chlorosulfonic acid → 3-acetyl-7-chlorosulfonyl-8-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine
反応式
[C:1]([N:4]1[CH2:10][CH2:9][C:8]2[CH:11]=[CH:12][C:13]([O:15][CH3:16])=[CH:14][C:7]=2[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[Cl:17][S:18](O)(=[O:20])=[O:19]>>[C:1]([N:4]1[CH2:5][CH2:6][C:7]2[CH:14]=[C:13]([O:15][CH3:16])[C:12]([S:18]([Cl:17])(=[O:20])=[O:19])=[CH:11][C:8]=2[CH2:9][CH2:10]1)(=[O:3])[CH3:2]参加物
3
実験手順
3-Acetyl-7-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine (2.3 g, 0.01 m) was added to chlorosulfonic acid (6 ml) which was stirred at 0°; the mixture was allowed to warm to 25° and stirred for 16 hours. The reaction was carefully poured into ice water and extracted with methylene chloride. The methylene chloride extracts were combined, washed, dried with magnesium sulfate and concentrated in vacuo to give 3-acetyl-7-chlorosulfonyl-8-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine, m.p. 153°-160°.
後処理
- temperatureto warm to 25°
- stirringstirred for 16 hours
- extractionextracted with methylene chloride
- washwashed
- dry with materialdried with magnesium sulfate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-fd3acbc775554dd6b808502b627656c7
- 出典データセット
- uspto-grants-1987_04
- 特許番号
- US04659706
反応ノート
読み込み中…