HRID1389131

反应详情

EQUATION

反应方程式

HRID 1389131 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of cyclohexyl pyrrol-2-yl ketone (17.7 g.) and 99% hydrazine hydrate (6.0 ml.) was heated under reflux in diethylene glycol (70 ml.) for 1.5 hours. The excess hydrazine hydrate and water were distilled off and the mixture was cooled. Potassium hydroxide (12.0 g.) was added portionwise and the mixture was then heated under reflux for 4 hours, cooled and poured into water (500 ml.). The mixture was extracted with ether (3×100 ml.) and the combined etheral extracts were washed with water (3×100 ml.) and dried over sodium sulphate. Evaporation of the ether gave an oil which was distilled to give 2-cyclohexylmethylpyrrole (11.3 g.), B.P. 137°-140° at 15 mm.

WORKUP

后处理

  1. temperaturewas heated
  2. distillationThe excess hydrazine hydrate and water were distilled off
  3. temperaturethe mixture was cooled
  4. additionPotassium hydroxide (12.0 g.) was added portionwise
  5. temperaturethe mixture was then heated
  6. temperatureunder reflux for 4 hours
  7. temperaturecooled
  8. additionpoured into water (500 ml.)
  9. extractionThe mixture was extracted with ether (3×100 ml.)
  10. washthe combined etheral extracts were washed with water (3×100 ml.)
  11. dry with materialdried over sodium sulphate
  12. customEvaporation of the ether
  13. customgave an oil which
  14. distillationwas distilled