HRID1252607

反应详情

EQUATION

反应方程式

HRID 1252607 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 7.29 g (0.13 mol) of potassium hydroxide in 500 ml of ethanol was added dropwise to a mixture of 60.8 g (0.13 mol) of 2-[[[[(2-chloroethyl)amino]carbonyl]amino]methyl]-5-(phenylmethoxy)-2-(phenylmethyl)-4(1H)-pyridinone and 1.3 l of ethanol. The reaction mixture was heated to reflux for three hours and the solvent evaporated in vacuo. The residue was purified by column chromatography on silica gel using a mixture of ethyl acetate and methanol (7:3) as eluent, yielding 23.1 g of product, which was further purified by recrystallization from acetonitrile, yielding 17.0 g of the title compound, melting point 190° C., dec.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for three hours
  3. customthe solvent evaporated in vacuo
  4. customThe residue was purified by column chromatography on silica gel using
  5. additiona mixture of ethyl acetate and methanol (7:3) as eluent