Reaktion #465489

Reaktionsgleichung

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

dimethylamine

dimethylamine

→

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

Ausbeute 8.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto evaporate
2. 2
   Sonstigethe residue was chromatographed on silica gel with ethyl acetate/hexane 1:1
3. 3
   SonstigeThe polar fractions were chromatographed twice on silica gel with ethyl acetate/hexane 2:3 and 1:1 as the eluent

Vorschrift

2.5 g (0.007 mol) of 4-amino-N-(2-bromo-6-methylamino-pyridin-4-yl)-benzenesulfonamide were stirred with 80 ml of dimethylamine in an autoclave at 160° C. for 7 hours. The residual dimethylamine was left to evaporate and the residue was chromatographed on silica gel with ethyl acetate/hexane 1:1, then 2:1 and finally 3:1. The polar fractions were chromatographed twice on silica gel with ethyl acetate/hexane 2:3 and 1:1 as the eluent. There was obtained 0.175 g (8%) of 4-amino-N-(2-dimethylamino-6-methylamino-pyridin-4-yl)-benzenesulfonamide as beige crystals: MS (ISP): me/e=322 (C14H20N5O2S+).

Quelle