HRID477829

反应详情

EQUATION

反应方程式

HRID 477829 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 22.2 g of ethyl 2,3,4,5-tetrafluorobenzoate, 22.2 g of 2-(N-ethoxycarbonyl-N-methylaminomethyl)morpholine and 8.4 g of sodium hydrogen carbonate in 130 ml of acetonitrile is refluxed for 7 hours. The reaction mixture is concentrated under reduced pressure, to the obtained residue is added 100 ml of chloroform and the solution is washed with water. After drying over anhydrous magnesium sulfate, the chloroform is distilled off under reduced pressure and the residue is puiified by chromatography on silica gel to give 29.0 g of ethyl 4-[2-(N-ethoxycarbonyl-N-methylaminomethyl)morpholino]-2,3,5-trifluorobenzoate in 72% yield, as an oily substance.

WORKUP

后处理

  1. temperatureis refluxed for 7 hours
  2. concentrationThe reaction mixture is concentrated under reduced pressure, to the obtained residue
  3. additionis added 100 ml of chloroform
  4. washthe solution is washed with water
  5. dry with materialAfter drying over anhydrous magnesium sulfate
  6. distillationthe chloroform is distilled off under reduced pressure