HRID1252628

反应详情

EQUATION

反应方程式

HRID 1252628 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.5 g of p-toluenesulfonic acid, 6.26 g of 2-(1-hydroxy-1-methoxymethyl)-5-(phenylmethoxy)-4(1H)-pyridinone and 8.35 g of carbethoxymethylenetriphenylphosphorane were stirred for 3 hours in 100 ml of dioxane at 70° C. A clear, dark-colored solution was formed. Evaporation of the solvent in vacuo yielded an oily residue of the title compound and triphenylphosphine oxide. The residue was dissolved in 30 ml of isopropanol and crystals of product began to separate. After standing in a refrigerator overnight, the crystals were filtered off, washed with ether and recrystallized from isopropanol. Yield: 5.72 g, melting point 188° C.

WORKUP

后处理

  1. customA clear, dark-colored solution was formed
  2. customEvaporation of the solvent in vacuo