HRID1252607
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction mixture was heated
- temperatureto reflux for three hours
- customthe solvent evaporated in vacuo
- customThe residue was purified by column chromatography on silica gel using
- additiona mixture of ethyl acetate and methanol (7:3) as eluent