HRID434576

反应详情

EQUATION

反应方程式

HRID 434576 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 50.0 g (0.31 mol) of 2,4-difluoronitrobenzene II, 56.1 g (0.32 mol) of diethylmethylmalonate and 400 ml of dimethylformamide are vigorously stirred. To the stirring mixture is added 13.1 g (0.33 mol) sodium hydroxide in one portion at 25° C., cooling with ice to keep the temperature of the reaction mixture at 25°-30° C. during the first hour. Thereafter, stirring is maintained for 3.5 hours, then 800 ml of water is added, the organic layers removed, and the aqueous layer extracted with three 180-ml portions of ethyl acetate-water.

WORKUP

后处理

  1. temperaturecooling with ice
  2. customat 25°-30° C.
  3. stirringThereafter, stirring
  4. temperatureis maintained for 3.5 hours
  5. customthe organic layers removed
  6. extractionthe aqueous layer extracted with three 180-ml portions of ethyl acetate-water