Reaktion #465480

Reaktionsgleichung

N-[4-(3,5-diamino-phenylsulfamoyl)-phenyl]-acetamide

ammonium chloride

→

4-amino-N-(3,5-diamino-phenyl)benzenesulfonamide

Ausbeute 55.0%

Lösungsmittel

NaOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux for 15 hours
2. 2
   Extraktionextracted twice with 100 ml of ethyl acetate each time
3. 3
   WaschenThe combined organic phases were washed with saturated sodium chloride solution
4. 4
   Trocknendried over MgSO4
5. 5
   SonstigeAfter removal of the solvent the residue
6. 6
   Sonstigewas chromatographed on aluminium oxide (neutral, activity 1), firstly with 5%

Vorschrift

0.105 g (0.00033 mol) of N-[4-(3,5-diamino-phenylsulfamoyl)-phenyl]-acetamide was dissolved in 6.5 ml of 1N NaOH and boiled at reflux for 15 hours. The reaction mixture was treated with 50 ml of saturated ammonium chloride solution and extracted twice with 100 ml of ethyl acetate each time. The combined organic phases were washed with saturated sodium chloride solution and dried over MgSO4. After removal of the solvent the residue was chromatographed on aluminium oxide (neutral, activity 1), firstly with 5% and then 10% methanol in dichloromethane. There was obtained 0.05 g (55%) of 4-amino-N-(3,5-diamino-phenyl)benzenesulfonamide as a beige solid; m.p.: 188-190° C.

Quelle