تفاعل #470395

معادلة التفاعل

1-fluoro-2-nitrobenzene

2-aminobiphenyl

potassium fluoride

→

product

المردود 91.1%

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

المردود 91.1%

ظروف التفاعل

المعالجة

1. 1
   أخرىwas prepared in a 100 mL round bottom flask
2. 2
   أخرىThe flask was evacuated
3. 3
   درجة الحرارةThe reaction mixture was cooled
4. 4
   workup.ADDITIONethyl acetate and water were added
5. 5
   أخرىThe layers were separated
6. 6
   استخلاصthe aqueous layer was extracted with ethyl acetate
7. 7
   تجفيفThe organic layers were dried over magnesium sulfate
8. 8
   ترشيحfiltered
9. 9
   أخرىevaporated
10. 10
    أخرىThe residue was preabsorbed onto Celite
11. 11
    أخرىpurified by column chromatography
12. 12
    غسيلeluting with 0, 2, and 5% ethyl acetate/hexanes

الإجراء التجريبي

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.

المصدر