HRID365006

反应详情

EQUATION

反应方程式

HRID 365006 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-(4-dimethylaminomethyl-2-pyridylmethylthio)ethylamine (1 g) and 2-nitroamino-5-(5,6-dimethyl-3-pyridylmethyl)-4-pyrimidone (1.11 g) in pyridine (3 ml) was heated under reflux for 5 hours and evaporated to dryness in vacuo. The residue was purified by chromatography on silica gel eluted with 20% methanol/chloroform followed by recrystallisation from acetonitrile/water 1:1 to give 2-[2-(4-dimethylaminomethyl-2-pyridylmethylthio)ethylamino]-5-(5,6-dimethyl-3-pyridylmethyl)-4-pyrimidone (0.72 g) m.p. 72°-78°.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 5 hours
  3. customevaporated to dryness in vacuo
  4. customThe residue was purified by chromatography on silica gel
  5. washeluted with 20% methanol/chloroform
  6. customfollowed by recrystallisation from acetonitrile/water 1:1