HRID66783

反应详情

EQUATION

反应方程式

HRID 66783 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.05 mol of 4-fluorophenylhydrazine hydrochloride and 0.05 mol of N-(3-oxocyclohexyl)acetamide in 75 ml of glacial HOAc was stirred and heated on the steam bath. At 80°-90° an exothermic reaction occurred and the source of heat was removed until the temperature had fallen to 85°. After an additional 4-5 hr at 85°-90°, the warm mixture was poured into H2O and the gummy insolubles triturated until solid. The filtered solid was washed thoroughly with H2O and then with Et2O until the washings were essentially colorless. The crude product was recrystallized from ethanol to give the title compound, mp 209°-210°.

WORKUP

后处理

  1. temperatureheated on the steam bath
  2. customAt 80°-90° an exothermic reaction
  3. temperaturethe source of heat
  4. customwas removed until the temperature
  5. customhad fallen to 85°
  6. additionthe warm mixture was poured into H2O
  7. customthe gummy insolubles triturated until solid
  8. washThe filtered solid was washed thoroughly with H2O
  9. customThe crude product was recrystallized from ethanol