반응 #1904044

반응 방정식

4-bromoiodobenzene

2-phenylindole

potassium carbonate

o-dichlorobenzene

→

1-(4-bromophenyl)-2-phenylindole

수율 50.1%

용매

hexane ethyl acetate

Toluene

반응 조건

후처리

1. 1
   온도refluxed
2. 2
   온도heated
3. 3
   workup.STIRRINGunder stirring at 60° C.
4. 4
   여과insoluble matter was filtered off
5. 5
   기타dried
6. 6
   workup.ADDITIONHexane was added to the residue
7. 7
   여과was filtered off
8. 8
   기타condensed
9. 9
   기타recrystallized with a mixed solvent of hexane/ethyl acetate

실험 절차

50.0 g (177 mmole) of 4-bromoiodobenzene, 28.5 g (177 mmole) of 2-phenylindole, 30.5 g (221 mmole) of potassium carbonate, 18.7 g of copper powder, and 150 ml of o-dichlorobenzene were put in a 500 ml three-necked flask, and refluxed with stirring for 25 hours under nitrogen flow. Toluene was added to the reaction mixture heated under stirring at 60° C., and insoluble matter was filtered off. The filtrate was vacuum dried. Hexane was added to the residue and deposited crystal was filtered off. The filtrate was condensed, and refined by silica gel column chromatography (eluent:hexane/ethyl acetate: 50/1), recrystallized with a mixed solvent of hexane/ethyl acetate to give 25.7 g of a white crystal of 1-(4-bromophenyl)-2-phenylindole (yield: 50.1%).

출처