HRID1108293

反应详情

EQUATION

反应方程式

HRID 1108293 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

5.0 g (35 mmol) of 2,4-difluorobenzaldehyde are dissolved with 5.7 g (35 mmol) of 2-methoxyethyl acetoacetate in 100 ml of isopropanol. A freshly prepared solution of 1.0 ml of piperidine and 0.5 ml of glacial acetic acid in 5 ml of isopropanol is added and the mixture is stirred at 40° C. overnight. The mixture is concentrated, the residue is taken up in toluene, this mixture is concentrated again and the residue is purified by filtration over 100 ml of silica gel (mobile phase: toluene/ethyl acetate 100:1) to give 5 g of the target compound as a yellow oil, which is immediately reacted further.

WORKUP

后处理

  1. concentrationThe mixture is concentrated
  2. concentrationthis mixture is concentrated again
  3. filtrationthe residue is purified by filtration over 100 ml of silica gel (mobile phase: toluene/ethyl acetate 100:1)