HRID1241221

反应详情

EQUATION

反应方程式

HRID 1241221 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

9-Fluorenone (200 g, 1.1 mol, from Aldrich, Milwaukee, Wis.) and hydrazine monohydrate (160 ml, 3.3 mol, from Aldrich, Milwaukee, Wis.) were dissolved in 1000 ml of 2-propanol in a 2000 ml 2-neck round bottom flask equipped with a reflux condenser and a mechanical stirrer. Concentrated hydrochloric acid (4 ml) was then added, and the mixture was refluxed for one hour. The mixture was cooled slowly to room temperature, and the crude solid product was harvested by filtration. The solid was washed with isopropanol and then recrystallized from dioxane to obtain 150 g (74% yield) of 9-fluorenone hydrazone.

WORKUP

后处理

  1. customequipped with a reflux condenser and a mechanical stirrer
  2. temperaturethe mixture was refluxed for one hour
  3. filtrationthe crude solid product was harvested by filtration
  4. washThe solid was washed with isopropanol
  5. customrecrystallized from dioxane