反応 #52114

反応方程式

HCl

biphenyl

benzoyl chloride

aluminum trichloride

→

dibenzoyl biphenyl

溶媒

nitrobenzene

反応条件

後処理

1. 1
   その他equipped with a water condenser
2. 2
   その他During the reaction
3. 3
   温度the temperature increased from 30° C. to 55° C
4. 4
   workup.STIRRINGwhile stirring
5. 5
   その他The organic layer was separated
6. 6
   workup.ADDITIONpoured into a blender and 500 mL n-hexane
7. 7
   workup.ADDITIONwas added
8. 8
   workup.STIRRINGThe mixture was vigorously stirred for 5 minutes
9. 9
   ろ過filtered
10. 10
    洗浄The solid was washed with n-hexane
11. 11
    乾燥The thus-produced dibenzoyl biphenyl was dried
12. 12
    その他recrystalized twice in chloroform

実験手順

The photoinitiator dibenzoyl biphenyl was prepared by placing 200 mL nitrobenzene, 38.5 g (0.25 mole) biphenyl, and 140.6 g (1.00 mole) benzoyl chloride into a 1 liter 3-necked flask equipped with a water condenser. While stirring, 160 g (1.2 mole) aluminum trichloride was added slowly over a period of about 30 minutes. During the reaction, the temperature increased from 30° C. to 55° C. The color changed from yellowish to light brown, then reddish. The flask was kept in a water bath at a temperature of 55° C. to 60° C. for 3 hours while stirring. The reaction mixture was then cooled to 35° C. The reaction mixture was poured into 1.2 L of 8% HCl solution with vigorous stirring. The organic layer was separated and poured into a blender and 500 mL n-hexane was added. The mixture was vigorously stirred for 5 minutes and then filtered. The solid was washed with n-hexane. The thus-produced dibenzoyl biphenyl was dried and recrystalized twice in chloroform.

出典