Reaktion #969897

ord-2d6f4484f9314edbbd2af6e7144af055

Lösungsmittel

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturis maintained at that temperature for 1.5 hours
  2. 2
    TemperaturAfter cooling
  3. 3
    Sonstigethe stirred reaction solution
  4. 4
    SonstigeA precipitate is formed which
  5. 5
    Filtrationis rapidly filtered off
  6. 6
    Waschenrinsed with toluene
  7. 7
    Trocknendried at 40° C. in vacuo in the presence of KOH pellets

Vorschrift

Dimethylformamide (0.152 mol) is added dropwise to a suspension of 2-amino-5-methoxybenzenesulphonic acid (0.152 mol) in thionyl chloride (0.763 mol). The reaction mixture is heated very gradually to 70° C. and is maintained at that temperature for 1.5 hours. After cooling, the stirred reaction solution is treated by the addition of 20 ml of toluene. A precipitate is formed which is rapidly filtered off, rinsed with toluene and then dried at 40° C. in vacuo in the presence of KOH pellets, to yield the title product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08236790B2uspto-grants-2012_08