反応 #2439931

反応方程式

2,7-dibromofluorenone

acetic acid

→

2,7-dibromo-9,9′-spirobifluorene

収率 60.0%

溶媒

ether

反応条件

後処理

1. 1
   workup.DISTILLATIONEther is distilled away under reduced pressure
2. 2
   workup.ADDITIONby adding
3. 3
   温度Thereafter, the solution is refluxed for 1 hr
4. 4
   ろ過by filtering precipitate by suction
5. 5
   洗浄by washing with water
6. 6
   その他recrystallizing with methanol

実験手順

According to a method similar to that of synthesis example 3, 2,7-dibromofluorenone (0.1 mol) and 2-biphenyl magnesium bromide are agitated in ether for 3 hr, followed by cooling to room temperature, further followed by slowly adding 50 ml of acetic acid. Ether is distilled away under reduced pressure, followed by adding thereto substantially 5 ml of HCl. Thereafter, the solution is refluxed for 1 hr, followed by filtering precipitate by suction, further followed by washing with water and recrystallizing with methanol. Thereby, 2,7-dibromo-9,9′-spirobifluorene is obtained (yield: 60%).

出典