HRID1248314

反应详情

EQUATION

反应方程式

HRID 1248314 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 2-formyl-3-(3-methoxyphenyl)propionate (10 g) was added dropwise to a stirred and boiling mixture of sodium methoxide (from 1.15 g sodium) and nitroguanidine (25% wet, 5.5 g) in methanol (250 ml) and the mixture was heated under reflux for 20 hours and evaporated to dryness. The residue was dissolved in water (100 ml), the solution was extracted with ether and the aqueous phase was adjusted to pH 4: the solid which separated was recrystallized from ethanol to give 2-nitroamino-5-(3-methoxybenzyl)-4-pyrimidone (3.41 g, 29%), m.p 178°-9°.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 20 hours
  3. customevaporated to dryness
  4. dissolutionThe residue was dissolved in water (100 ml)
  5. extractionthe solution was extracted with ether
  6. customthe solid which separated
  7. customwas recrystallized from ethanol