HRID597541

反应详情

EQUATION

反应方程式

HRID 597541 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
115 °C

PROCEDURE

实验过程

Cyclohexanone (2.0 ml., 0.020 mole), phenylhydrazine hydrochloride (2.88 g., (0.020 mole) and 6.0 ml. of freshly distilled pyridine are combined, heated at reflux (115° C) for 3 hours, then allowed to cool to room temperature and allowed to stir overnight. About 25 ml. of water is added and the precipitated solids are collected by decantation. After washing again with water, the solids are dissolved in a mixture of 20 ml. of ethanol and 5 ml. of water and set aside. The resulting crystals are collected by filtration, washed with aqueous ethanol and dried to afford 2.65 g. (77.5% of theory) of the title compound, M.P. 119°-120° C. A mixture of the product and an authentic sample of 1,2,3,4-tetrahydrocarbazole also melted at 119°-120° C.

WORKUP

后处理

  1. temperatureheated
  2. temperatureto cool to room temperature
  3. customthe precipitated solids are collected by decantation
  4. washAfter washing again with water
  5. dissolutionthe solids are dissolved in a mixture of 20 ml
  6. filtrationThe resulting crystals are collected by filtration
  7. washwashed with aqueous ethanol
  8. customdried
  9. customto afford 2.65 g