반응 #11290

반응 방정식

diphenylisobenzofuran

5-bromoacenaphthylene

→

3-bromo-7,12-diphenylbenzo[k]fluoranthene

수율 78.3%

용매

toluene

반응 조건

후처리

1. 1
   workup.DISTILLATIONThe solvent was distilled off in vacuum
2. 2
   workup.DISSOLUTIONafter which the residue was dissolved in 500 ml of acetic acid
3. 3
   workup.ADDITIONAn aqueous 40% hydrobromic acid solution, 50 cm3, was added to the solution, which
4. 4
   온도After cooling to room temperature
5. 5
   여과the precipitate was collected by filtration
6. 6
   기타This was purified by silica gel chromatography
7. 7
   workup.ADDITIONa mixture of toluene and hexane as an extracting solvent

실험 절차

5 g (18.5 mmol) of diphenylisobenzofuran and 4.3 g (18.5 mmol) of 5-bromoacenaphthylene in toluene were agitated for 24 hours at the reflux temperature. The solvent was distilled off in vacuum, after which the residue was dissolved in 500 ml of acetic acid. An aqueous 40% hydrobromic acid solution, 50 cm3, was added to the solution, which was heated at 80° C. for one hour. After cooling to room temperature, the precipitate was collected by filtration. This was purified by silica gel chromatography using a mixture of toluene and hexane as an extracting solvent, yielding 7 g of 3-bromo-7,12-diphenylbenzo[k]fluoranthene having a yellowish white color.

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