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 during 5 minutes with stirring and ice-cooling with a solution of 1.52 g. of sodium nitrite in 10 ml. of water. The solution was stirred at 0° C. for 30 minutes and 14.6 g. of diethylamine were then added. After stirring with ice-cooling for 2 hours, the precipitate was removed by filtration with suction, washed with water and recrystallized from methanol, whereby there was obtained 2,4-diamino-5-[4-(3,3-diethyl-1-triazeno)-3,5-dimethoxy-benzyl]-pyrimidine having a melting point of 196°-197° C. (decomposition).

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