HRID441347

反应详情

EQUATION

反应方程式

HRID 441347 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

Potassium 2,4-dichlorophenate is prepared by dissolving 6.5 g. (0.04 mole) of 2,4-dichlorophenol and 2.6 g. (0.04 mole) of 85% potassium hydroxide in 30 ml. of methanol and removing the solvent under reduced pressure. The solid residue is dissolved in 60 ml. of sulfolane and 6.2 g. (0.04 mole) of 3-methyl-4-nitrofluorobenzene is added. The resulting solution is heated at 85° C. for 3 hours then at 150° C. for 1 hour, cooled, diluted with water and extracted with ether/benzene. The extract is dried and the solvent removed. The residue is dissolved in hot isopropanol and on cooling 8.2 g. (69%) of 2,4-dichloro-3'-methyl-4'-nitrodiphenyl ether (m.p. 72.5°-73.5° C.) separated and is isolated by filtration.

WORKUP

后处理

  1. dissolutionby dissolving 6.5 g
  2. customof methanol and removing the solvent under reduced pressure
  3. dissolutionThe solid residue is dissolved in 60 ml
  4. temperaturecooled
  5. extractionextracted with ether/benzene
  6. customThe extract is dried
  7. customthe solvent removed
  8. dissolutionThe residue is dissolved in hot isopropanol
  9. temperatureon cooling 8.2 g
  10. custom(69%) of 2,4-dichloro-3'-methyl-4'-nitrodiphenyl ether (m.p. 72.5°-73.5° C.) separated
  11. customis isolated by filtration