HRID1709691

反应详情

EQUATION

反应方程式

HRID 1709691 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3,4,5-trichloronitrobenzene (13.55 g, 59 mmol), potassium fluoride (4.65 g, 80 mmol) and dimethylformamide (DMF; 66 ml) is heated at 140° for 15 hours. An additional 2.5 g of potassium fluoride is added and the mixture is stirred an additional 15 hours at 140°. The reaction mixture is poured into water and extracted with ether. The combined organic layers are washed with water and with brine and filtered, and the solvent is removed to give a dark solid, which is purified by column chromatography to give 3,5-dichloro-4-fluoronitrobenzene, a yellow powder.

WORKUP

后处理

  1. temperatureis heated at 140° for 15 hours
  2. extractionextracted with ether
  3. washThe combined organic layers are washed with water and with brine
  4. filtrationfiltered
  5. customthe solvent is removed
  6. customto give a dark solid, which
  7. customis purified by column chromatography