HRID903370

反应详情

EQUATION

反应方程式

HRID 903370 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Nitroguanidine (9.10 g) was added to a solution of sodium methoxide (from 2.22 g sodium) in methanol (100 ml) and the mixture was heated under reflux for 45 minutes, ethyl 2-formyl-3-(1-naphthyl)propionate (16.05 g) was added and the mixture was heated under reflux for 20 hours and evaporated to dryness. The residue was poured into water and the mixture was extracted with chloroform and the pH of the residual aqueous phase was adjusted to 4 with acetic acid. The solid which precipitated was recrystallised from acetic acid to give 2-nitroamino-5-(1-naphthylmethyl)-4-pyrimidone, m.p. 226°-7°.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 45 minutes
  3. temperaturethe mixture was heated
  4. temperatureunder reflux for 20 hours
  5. customevaporated to dryness
  6. additionThe residue was poured into water
  7. extractionthe mixture was extracted with chloroform
  8. customThe solid which precipitated
  9. customwas recrystallised from acetic acid