HRID127204

反应详情

EQUATION

反应方程式

HRID 127204 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

An equimolar mixture of 2-nitroamino-5-(2-methoxy-4-pyridylmethyl)-4-pyrimidone and 2-(2-thiazolylmethylthio) ethylamine was heated under reflux in ethanol for 18 hours. The solid which crystallised out on cooling was purified by column chromatography on silica gel and recrystallisation from 2-propanol-ethanol to give 2-[2-(2-thiazolylmethylthio)ethylamino]-5-(2-methoxy-4-pyridylmethyl)-4-pyrimidone, m.p. 105.5-106.5° in 41% yield. The latter compound was heated under reflux in 2N hydrogen chloride in ethanol for 24 hours to give 2-[2-(2-thiazolylmethylthio)ethylamino]-5-(2-hydroxy-4-pyridylmethyl)-4-pyrimidone monohydrochloride, m.p. 169-173°.

WORKUP

后处理

  1. temperaturewas heated
  2. customThe solid which crystallised out
  3. temperatureon cooling
  4. customwas purified by column chromatography on silica gel and recrystallisation from 2-propanol-ethanol