HRID903363

反应详情

EQUATION

反应方程式

HRID 903363 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethyl 2-formyl-3-(6-methyl-3-pyridyl)-propionate (1.55 g) in methanol (20 ml) was added to a stirred solution of sodium methoxide (from 0.161 g sodium) in methanol (20 ml). Dried nitroguanidine (0.73 g) was added and the mixture was heated under reflux overnight and evaporated to dryness. The residue was dissolved in water (50 ml) and the solution was extracted with chloroform and the aqueous phase was adjusted to pH 5 with acetic acid. The solid which precipitated was filtered off and recrystallised from methanol-acetic acid to give 2-nitroamino-5-(6-methyl-3-pyridylmethyl)-4-pyrimidone (0.5 g, 27%), m.p. 215°-6° (decomp).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux overnight
  3. customevaporated to dryness
  4. dissolutionThe residue was dissolved in water (50 ml)
  5. extractionthe solution was extracted with chloroform
  6. customThe solid which precipitated
  7. filtrationwas filtered off
  8. customrecrystallised from methanol-acetic acid