HRID903365

反应详情

EQUATION

反应方程式

HRID 903365 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Nitroguanidine (4.7 g) was added to a solution of sodium methoxide (prepared from 1.15 g sodium) in methanol (50 ml) and the mixture was heated under reflux for 45 minutes. Ethyl 2-formyl-3-(6-methoxy-3-pyridyl)propionate (10.7 g) was added and the mixture was heated under reflux for 24 hours and evaporated to dryness. The residue was dissolved in water and the solution was extracted with chloroform. The residual aqueous solution was adjusted to pH 5 with acetic acid, and the solid which precipitated was filtered off to give 2-nitroamino-5-(6-methoxy-3-pyridylmethyl)-4-pyrimidone, m.p. 183.5°-186°.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 45 minutes
  3. temperaturethe mixture was heated
  4. temperatureunder reflux for 24 hours
  5. customevaporated to dryness
  6. dissolutionThe residue was dissolved in water
  7. extractionthe solution was extracted with chloroform
  8. customthe solid which precipitated
  9. filtrationwas filtered off