Reaktion #698011

ord-4ba8021258cd47928f38a102acd51021

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturin reflux for 4 hours
  2. 2
    Sonstigethe precipitate which separated
  3. 3
    Filtrationwas filtered off
  4. 4
    SonstigeAfter drying the material on the suction
  5. 5
    Filtrationfilter
  6. 6
    Sonstigewas chromatographed on silica gel with 3% methanol with dichloromethane

Vorschrift

2.5 g (0.0069 mol) of N-[4-[3-(acetyl-methyl-amino)-phenylsulfamoyl]-phenyl]-acetamide were dissolved in 150 ml of 1N NaOH and boiled in reflux for 4 hours. Subsequently, the pH value was adjusted to 4 with 1N HCl and the precipitate which separated was filtered off. After drying the material on the suction filter was chromatographed on silica gel with 3% methanol with dichloromethane. There were obtained 1.64 g (85%) of 4-amino-N-(3-methylamino-phenyl)-benzenesulfonamide as a yellowish solid; m.p.: 134-135° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05998665uspto-grants-1999_12