反应 #470395

反应方程式

1-fluoro-2-nitrobenzene

2-aminobiphenyl

potassium fluoride

→

product

收率 91.1%

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

收率 91.1%

反应条件

后处理

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

实验过程

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.

来源