Reaktion #465482

Reaktionsgleichung

N-[3-(4-acetylamino-phenylsulfonylamino)-5-(acetyl-methyl-amino)-phenyl]-N-methyl-acetamide

HCl

→

4-amino-N-(3,5-bis-methylamino-phenyl)-benzenesulfonamide hydrochloride

Ausbeute 74.0%

Lösungsmittel

NaOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux for 2 hours
2. 2
   Extraktionextracted with ethyl acetate
3. 3
   Trocknenthe organic phase was dried over sodium sulfate
4. 4
   SonstigeAfter removal of the solvent the residue
5. 5
   workup.DISSOLUTIONwas dissolved in 4 ml of methanol
6. 6
   workup.ADDITIONtreated with 3 ml of 2M HCl
7. 7
   workup.ADDITIONAfter the addition of 7-8 ml of ethyl acetate the product
8. 8
   Sonstigeseparated out slowly
9. 9
   FiltrationIt was filtered off
10. 10
    Sonstigedried in a vacuum

Vorschrift

0.113 g (0.00026 mol) of N-[3-(4-acetylamino-phenylsulfonylamino)-5-(acetyl-methyl-amino)-phenyl]-N-methyl-acetamide was dissolved in 10 ml of 1N NaOH and boiled at reflux for 2 hours. The mixture was neutralized with 1N HCl, extracted with ethyl acetate and the organic phase was dried over sodium sulfate. After removal of the solvent the residue was dissolved in 4 ml of methanol and treated with 3 ml of 2M HCl. After the addition of 7-8 ml of ethyl acetate the product separated out slowly. It was filtered off and dried in a vacuum. There was obtained 0.085 g (74%) of 4-amino-N-(3,5-bis-methylamino-phenyl)-benzenesulfonamide hydrochloride (1:2.6) as a pink coloured amorphous solid. MS (ISN): me/e=305 (C14H17N4O2S-).

Quelle