反应详情

155.2 g (1 mol) of 2-dimethylamino-4,6-dihydroxypyrimidine are added while stirring to 1000 cc of 1N sodium hydroxide solution 1N and the mixture is heated to 50° over a short period. 170 g (1.1 mol) of diethyl sulphate are subsequently added dropwise, over the course of 2 hours, at 40°-45°. During the dropwise addition the pH value is kept at between 7.5 and 8.0 by further addition of 1N sodium hydroxide solution. Approximately 500 cc of 1N sodium hydroxide solution are additionally required. The mixture is stirred at 40° for 6 hours, filtered off, washed with a small amount of water and dried at 90° in a high vacuum. The compound may be recrystallized from benzene. M.P. 194°-195°. The aqueous phase may be extracted with chloroform in order to obtain better yields. The chloroform solution is dried with sodium sulphate and after evaporation crystals are obtained which may be recrystallized from benzene.

1. temperaturethe mixture is heated to 50° over a short period
2. additionDuring the dropwise addition the pH value
3. filtrationfiltered off
4. washwashed with a small amount of water
5. customdried at 90° in a high vacuum
6. customThe compound may be recrystallized from benzene
7. extractionThe aqueous phase may be extracted with chloroform in order
8. customto obtain better
9. customyields
10. dry with materialThe chloroform solution is dried with sodium sulphate
11. customafter evaporation crystals
12. customare obtained which
13. custommay be recrystallized from benzene