反应详情

(a)(i) Sodium (1.15 g) was dissolved in methanol (50 ml), and nitroguanidine (4.7 g) was added to the cooled solution. The mixture was refluxed for 45 minutes, ethyl 2-formyl-3-(3-pyridyl)propionate (9.3 g) was added portionwise and the mixture was refluxed for 45 hours and evaporated to dryness. Water was added to the residue and the mixture was extracted with chloroform. The aqueous phase was adjusted to pH 5 with acetic acid, and the solid which was precipitated was filtered off, washed and dried to give 2-nitroamino-5-(3-pyridylmethyl)-4-pyrimidone, m.p. 214.5°-216°, in 38% yield.

1. temperatureThe mixture was refluxed for 45 minutes
2. temperaturethe mixture was refluxed for 45 hours
3. customevaporated to dryness
4. additionWater was added to the residue
5. extractionthe mixture was extracted with chloroform
6. customthe solid which was precipitated
7. filtrationwas filtered off
8. washwashed
9. customdried