反应详情

A solution of 7 g. of 2,4-diamino-5-(4-amino-3,5-dimethoxy-benzyl)-pyrimidine dihydrochloride in 60 ml. of 1N hydrochloric acid and 40 ml. of water was treated over a period of 5 minutes with stirring and ice-cooling with a solution of 1.52 g. of sodium nitrite in 10 ml. of water. After stirring at 0° C. for 30 minutes, a solution of 1.43 g. of sodium azide in 20 ml. of water was added. The solution was stirred at 0° C. for 2 hours and then treated with sodium bicarbonate to obtain an alkaline reaction. After stirring at 0° C. for 1 hour, the precipitate was removed by filtration with suction, washed with water and recrystallized from methanol, whereby there was obtained 2,4-diamino-5-(4-azido-3,5-dimethoxy-benzyl)-pyrimidine having a melting point of 152° C. (decomposition).

1. temperatureice-cooling with a solution of 1.52 g
2. stirringAfter stirring at 0° C. for 30 minutes
3. stirringThe solution was stirred at 0° C. for 2 hours
4. customto obtain
5. customan alkaline reaction
6. stirringAfter stirring at 0° C. for 1 hour
7. customthe precipitate was removed by filtration with suction
8. washwashed with water
9. customrecrystallized from methanol