반응 #162256

반응 방정식

2,4-diphenylaniline

1-bromo-2-fluorobenzene

sodium

→

2,4-diphenyl-N-2-fluorophenylbenzenamine

수율 61.9%

용매

toluene

toluene

반응 조건

후처리

1. 1
   기타is removed
2. 2
   추출The reaction mixture is extracted with dichloromethane and water
3. 3
   workup.DISTILLATIONbeing distilled under reduced pressure
4. 4
   여과The resulting residence is filtered by silica gel column
5. 5
   workup.DISTILLATIONdistilled under reduced pressure again
6. 6
   기타Next, by re-crystallizing
7. 7
   여과filtering with dichloromethane and petroleum ether

실험 절차

2,4-diphenylaniline (12 mmol), 1-bromo-2-fluorobenzene (10 mmol), tris(dibenzylideneacetone)dipalladium(0) (0.15 mmol), (±)-2,2′-bis(diphenylphosphine)-1,1′-binaphthalene (0.3 mmol) and sodium tert-butoxie (14 mmol) are put in a two-neck round-bottom flask and dissolved in toluene (30 mL). Subsequently, the resulting solution is stirred in a bath under a temperature of about 100° C. for 24 hours. After completion of the reaction, toluene is removed. The reaction mixture is extracted with dichloromethane and water, and then being distilled under reduced pressure. The resulting residence is filtered by silica gel column and distilled under reduced pressure again. Next, by re-crystallizing and filtering with dichloromethane and petroleum ether, 2,4-diphenyl-N-2-fluorophenylbenzenamine (2.1 g) is yielded.

출처