反应详情

Nitroguanidine (6.05 g) was added to a solution of sodium methoxide (prepared from 1.45 g sodium) in dry methanol (65 ml) and the mixture was heated under reflux for 0.75 hours. Ethyl 3-(5,6-dimethyl-3-pyridyl)-2-formylpropionate (14.3 g) was added and the mixture was heated under reflux for 40 hours and evaporated to dryness. Water (40 ml) was added to the residue and the mixture was extracted with chloroform. The aqueous phase was adjusted to pH 6 with hydrochloric acid and the solid which separated was filtered off and recrystallised from dimethylformamideethanol to give 5-(5,6-dimethyl-3-pyridylmethyl)-2-nitroamino-4-pyrimidone, m.p. 212°-3°.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 0.75 hours
3. temperaturethe mixture was heated
4. temperatureunder reflux for 40 hours
5. customevaporated to dryness
6. additionWater (40 ml) was added to the residue
7. extractionthe mixture was extracted with chloroform
8. customthe solid which separated
9. filtrationwas filtered off
10. customrecrystallised from dimethylformamideethanol