HRID224884

反应详情

EQUATION

反应方程式

HRID 224884 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 refluxed for 45 minutes. Ethyl 2-formyl-3-(6-methoxy-3-pyridyl)propionate (10.7 g) was added and the mixture was refluxed for 34 hours and evaporated to a residue. This residue was dissolved in water and the solution was extracted with chloroform (subsequently discarded). The aqueous solution was adjusted to pH 5 with acetic acid, and the solid which precipitated out 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 refluxed for 45 minutes
  2. temperaturethe mixture was refluxed for 34 hours
  3. customevaporated to a residue
  4. dissolutionThis residue was dissolved in water
  5. extractionthe solution was extracted with chloroform (
  6. customthe solid which precipitated out
  7. filtrationwas filtered off