HRID661768

反应详情

EQUATION

反应方程式

HRID 661768 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

There were mixed 10.00 g (30.86 mmol) of 2,7-dibromofluorene, 15.05 g (123.45 mmol) of phenylboronic acid, 29.21 g (92.59 mmol) of barium hydroxide (Ba(OH)2.8H2O) and 0.71 g (0.62 mmol) of tetrakis(priphenylphosphine) palladium in an atmosphere of nitrogen. To the mixture, 200 mL of 1,4-dioxane and 33 mL of water were added at a room temperature. Temperature of the resultant mixture was raised up to 80° C., and the mixture was heated at 80° C. for 6 hours. Temperature of the mixture was cooled down to a room temperature, and 200 mL of toluene and 100 mL of a saturated solution of sodium chloride were added to the mixture. The obtained mixture was filtered, thereby obtaining a white solid. There was extracted 2,7-diphenyfluorene from the white solid with each 400 mL of hot THF three times. THF contained in the extract was distilled away, and the resultant solid was dried under a reduced pressure, thereby obtaining 7.94 g (yield: 80%) of 2,7-diphenyfluorene as a white solid.

WORKUP

后处理

  1. temperatureTemperature of the mixture was cooled down to a room temperature
  2. filtrationThe obtained mixture was filtered
  3. customobtaining a white solid
  4. extractionThere was extracted 2,7-diphenyfluorene from the white solid with each 400 mL of hot THF three times
  5. distillationwas distilled away
  6. customthe resultant solid was dried under a reduced pressure