Reaktion #46918
ord-26b8734ec46f438d851b80c723a17934
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturAfter cooling the mixture
- 2Einengenwas concentrated under reduced pressure
- 3workup.ADDITIONEther (50 mL) was added to the residue
- 4Sonstigethe precipitate was isolated by filtration
- 5WaschenThe pale yellow solid was washed with ether
- 6Sonstigedried
Vorschrift
A mixture of Example 1A (3.3 g, 10.1 mmol) and 4-aminobenzenesulfonamide (1.74 g, 10.1 mmol) in glacial acetic acid (75 mL) was heated to 100° C. for 48 hours. After cooling the mixture was concentrated under reduced pressure. Ether (50 mL) was added to the residue and the precipitate was isolated by filtration. The pale yellow solid was washed with ether and dried. 1H NMR (CDCl3) δ ppm 1.32 (3H), 2.20 (3H), 3.50 (2H), 4.27 (2H), 6.85 (1H), 7.30-7.90 (8H); MS (ESI) m/z m/z 462/464.