반응 #470395

반응 방정식

1-fluoro-2-nitrobenzene

2-aminobiphenyl

potassium fluoride

→

product

수율 91.1%

N-(2-nitrophenyl)biphenyl-2-amine

수율 91.1%

반응 조건

후처리

1. 1
   기타was prepared in a 100 mL round bottom flask
2. 2
   기타The flask was evacuated
3. 3
   온도The reaction mixture was cooled
4. 4
   workup.ADDITIONethyl acetate and water were added
5. 5
   기타The layers were separated
6. 6
   추출the aqueous layer was extracted with ethyl acetate
7. 7
   건조The organic layers were dried over magnesium sulfate
8. 8
   여과filtered
9. 9
   기타evaporated
10. 10
    기타The residue was preabsorbed onto Celite
11. 11
    기타purified by column chromatography
12. 12
    세척eluting with 0, 2, and 5% ethyl acetate/hexanes

실험 절차

A mixture of 1-fluoro-2-nitrobenzene (13.06 g, 92.6 mmol), 2-aminobiphenyl (31.3 g, 185.2 mmol), and potassium fluoride (8.1 g, 138.9 mmol) was prepared in a 100 mL round bottom flask. The flask was evacuated and replaced with nitrogen. The mixture was heated to 200° C. overnight. The reaction mixture was cooled and ethyl acetate and water were added. The layers were separated and the aqueous layer was extracted with ethyl acetate. The organic layers were dried over magnesium sulfate, filtered, and evaporated. The residue was preabsorbed onto Celite and purified by column chromatography eluting with 0, 2, and 5% ethyl acetate/hexanes. 24.5 g (91%) of product was obtained.

출처