تفاعل #52114

ord-ac15554799264828811d5492b04508e7

معادلة التفاعل

Cl
HCl
c1ccc(-c2ccccc2)cc1
biphenyl
O=C(Cl)c1ccccc1
benzoyl chloride
[Al+3].[Cl-].[Cl-].[Cl-]
aluminum trichloride
O=C(c1ccccc1)c1ccc(-c2ccc(C(=O)c3ccccc3)cc2)cc1
dibenzoyl biphenyl

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
35°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىequipped with a water condenser
  2. 2
    أخرىDuring the reaction
  3. 3
    درجة الحرارةthe temperature increased from 30° C. to 55° C
  4. 4
    workup.STIRRINGwhile stirring
  5. 5
    أخرىThe 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
    ترشيحfiltered
  10. 10
    غسيلThe solid was washed with n-hexane
  11. 11
    تجفيفThe thus-produced dibenzoyl biphenyl was dried
  12. 12
    أخرىrecrystalized twice in chloroform

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06852894B2uspto-grants-2005_02