HRID322814

反应详情

EQUATION

反应方程式

HRID 322814 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 50 g of diethyl 2-(2,5,6-trifluoro-3,4-bis(ethoxycarbonyl)phenyl)malonate were added 60 ml of conc. hydrochloric acid and 60 ml of acetic acid, and the mixture was refluxed overnight. The ethyl acetate in the reaction solution was distilled off under reduced pressure, and the solution was refluxed for 2 days. The acid in the reaction solution was distilled off, and hexane was added to the residue. The solid content was collected by filtration and dried to obtain 27 g of the title compound in crude form.

WORKUP

后处理

  1. temperaturethe mixture was refluxed overnight
  2. distillationThe ethyl acetate in the reaction solution was distilled off under reduced pressure
  3. temperaturethe solution was refluxed for 2 days
  4. distillationThe acid in the reaction solution was distilled off
  5. additionhexane was added to the residue
  6. filtrationThe solid content was collected by filtration
  7. customdried