HRID1733405

反应详情

EQUATION

反应方程式

HRID 1733405 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,5-dichlorobenzoic acid (5 g) and 3,5-diisopropylphenol (4.66 g) were dissolved in dry xylene and the solution placed under dry oxygen-free nitrogen. Sodium hydride (1.25 g) was added as a suspension in petroleum ether. Cuprous bromide was added and the solution refluxed for 5 hours and cooled. The xylene was removed by low pressure distillation. The remaining solid was acidified with dilute hydrochloric acid and extracted with diethyl ether. The ethereal layer was separated, dried and distilled under low pressure to give an oil. The oil was dissolved in petroleum ether (30°-40° ). Standing gave a crystalline solid, which was recrystallised from hexane to give the title compound (4.3 g), mp 129°-130° C.

WORKUP

后处理

  1. temperaturethe solution refluxed for 5 hours
  2. temperaturecooled
  3. customThe xylene was removed by low pressure distillation
  4. extractionextracted with diethyl ether
  5. customThe ethereal layer was separated
  6. customdried
  7. distillationdistilled under low pressure
  8. customto give an oil
  9. customStanding gave a crystalline solid, which
  10. customwas recrystallised from hexane