Chlorosulfonic acid → 3-acetyl-7-chlorosulfonyl-8-methoxy-2,3,4,5-tetrahydro-1H-3-benzazepine
Reaktionsgleichung
[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]Komponenten
3
Versuchsvorschrift
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°.
Aufarbeitung
- temperatureto warm to 25°
- stirringstirred for 16 hours
- extractionextracted with methylene chloride
- washwashed
- dry with materialdried with magnesium sulfate
- concentrationconcentrated in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-9902e1c84c54472593c030c86f299233
- Quelldatensatz
- uspto-grants-1989_04
- Patentnummer
- US04824839
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