Reaktion #423975
ord-d2c4ba86e215421a88ec4f5efb1dd629
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
150°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Sonstigeprepared
- 2Sonstigeafter which time, solvent was removed on a rotary evaporator, and 10 mL of Dichloromethane and 50 mL of methanol
- 3workup.ADDITIONwere added
- 4TemperaturThe slurry was heated
- 5Temperaturto reflux
- 6Filtrationfiltered while hot,
- 7Sonstigeresulting in 4.6 g (69.7%) of N-(3-(3,5-dimethoxyphenylamino)quinoxalin-2-yl)-3-nitrobenzenesulfonamide MS (EI) m/z for C22H19N5O6S
Vorschrift
A flask was charged with N-(3-chloroquinoxalin-2-yl)-3-nitrobenzenesulfonamide (5 g, 13.7 mmol), prepared using procedures similar to those in Example 1, 3,5-dimethoxyaniline (4.2 g, 27.4 mmol), and 80 mL of xylene. The reaction mixture was stirred under an N2 atmosphere at 150° C. for 3 hours, after which time, solvent was removed on a rotary evaporator, and 10 mL of Dichloromethane and 50 mL of methanol were added. The slurry was heated to reflux and filtered while hot, resulting in 4.6 g (69.7%) of N-(3-(3,5-dimethoxyphenylamino)quinoxalin-2-yl)-3-nitrobenzenesulfonamide MS (EI) m/z for C22H19N5O6S: 482.2 (MH+).