HRID1093030

反应详情

EQUATION

反应方程式

HRID 1093030 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
168 °C

PROCEDURE

实验过程

Subsequently, in a stream of argon, 500 mL of diethylene glycol was added to 16.8 g (92.6 mmol) of 4-azafluorene-9-one and 25 mL (370 mmol) of hydrazine monohydrate, and was heated and stirred at 168° C. for 3 hours. After the reaction liquid was cooled to room temperature, an aqueous solution of sodium chloride was added to the reaction liquid, and then, was extracted with ethyl acetate. The organic phase was washed with water, dried over sodium sulfate and concentrated, to thereby obtain 15.3 g of 4-azafluorene (99% yield).

WORKUP

后处理

  1. temperaturewas heated
  2. customAfter the reaction liquid
  3. temperaturewas cooled to room temperature
  4. extractionwas extracted with ethyl acetate
  5. washThe organic phase was washed with water
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated