Reaktion #423975

ord-d2c4ba86e215421a88ec4f5efb1dd629

Lösungsmittel

Reaktionsbedingungen

Temperatur
150°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeprepared
  2. 2
    Sonstigeafter which time, solvent was removed on a rotary evaporator, and 10 mL of Dichloromethane and 50 mL of methanol
  3. 3
    workup.ADDITIONwere added
  4. 4
    TemperaturThe slurry was heated
  5. 5
    Temperaturto reflux
  6. 6
    Filtrationfiltered while hot,
  7. 7
    Sonstigeresulting 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+).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08889664B2uspto-grants-2014_11