Reaktion #430557

Reaktionsgleichung

5-Dimethylamino-1-naphthalenesulphonyl chloride

5-amino-2,4-dimethoxypyrimidine

→

5-dimethylamino-N-(2,4-dimethoxy-5-pyrimidinyl)-1-naphthalenesulphonamide

Ausbeute 72.2%

Lösungsmittel

Pyridine

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was then heated at 80° C. for 5 hours
2. 2
   SonstigeVolatile material was removed by evaporation
3. 3
   Sonstigethe residue was purified by elution with dichloromethane through a silica gel Mega Bond Elut column

Vorschrift

5-Dimethylamino-1-naphthalenesulphonyl chloride (0.296 g) and 5-amino-2,4-dimethoxypyrimidine (0.155 g) were mixed together as solids. Pyridine (10 mls) was added and the solution was stirred at 0° C. for 30 minutes. The mixture was then heated at 80° C. for 5 hours. Volatile material was removed by evaporation and the residue was purified by elution with dichloromethane through a silica gel Mega Bond Elut column to give 5-dimethylamino-N-(2,4-dimethoxy-5-pyrimidinyl)-1-naphthalenesulphonamide (0.28 g), m.p. 201° C.; 1H NMR (d6 -DMSO): 2.85 (s, 6H), 3.1 (s, 3H), 3.8 (s, 3H), 7.3 (d, 1H), 7.55 (q, 2H); 7.95 (d, 1H), 8.05 (s, 1H), 8.30 (d, 1H), 8.48 (d, 1H), 9.85 (s, 1H); mass spectrum (+ve CI): 389 (M+H)+.

Quelle