反応 #470395

反応方程式

1-fluoro-2-nitrobenzene

2-aminobiphenyl

potassium fluoride

→

product

収率 91.1%

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

収率 91.1%

反応条件

後処理

1. 1
   その他was prepared in a 100 mL round bottom flask
2. 2
   その他The flask was evacuated
3. 3
   温度The reaction mixture was cooled
4. 4
   workup.ADDITIONethyl acetate and water were added
5. 5
   その他The layers were separated
6. 6
   抽出the aqueous layer was extracted with ethyl acetate
7. 7
   乾燥The organic layers were dried over magnesium sulfate
8. 8
   ろ過filtered
9. 9
   その他evaporated
10. 10
    その他The residue was preabsorbed onto Celite
11. 11
    その他purified by column chromatography
12. 12
    洗浄eluting with 0, 2, and 5% ethyl acetate/hexanes

実験手順

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.

出典