Reaktion #698018

Reaktionsgleichung

hydrogen

4-amino-N-(2-bromo-6-methylamino-pyridin-4-yl)-benzenesulfonamide

→

4-amino-N-(2-methylamino-pyridin-4-yl)-benzenesulfonamide

Ausbeute 57.0%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe catalyst was filtered off
2. 2
   Einengenthe filtrate was concentrated
3. 3
   workup.DISSOLUTIONthe residue was dissolved in 10 ml of 1N NaOH
4. 4
   Filtrationfiltered
5. 5
   SonstigeThe precipitate which separated slowly
6. 6
   Filtrationwas filtered off under suction
7. 7
   Waschenrinsed
8. 8
   Sonstigedried in a high vacuum

Vorschrift

0.5 g (0.0014 mol) of 4-amino-N-(2-bromo-6-methylamino-pyridin-4-yl)-benzenesulfonamide was dissolved in 25 ml of ethanol, treated with 0.05 g of Pd/C and hydrogenated with hydrogen gas under normal pressure for 1 hour. The catalyst was filtered off, the filtrate was concentrated and the residue was dissolved in 10 ml of 1N NaOH, filtered and the filtrate was then adjusted pH 8 by means of 1N HCl. The precipitate which separated slowly was filtered off under suction, rinsed and dried in a high vacuum. There was obtained 0.22 g (57%) of 4-amino-N-(2-methylamino-pyridin-4-yl)-benzenesulfonamide as white crystals; m.p.: >261° C. (dec).

Quelle