반응 #75287

반응 방정식

4-bromo-2-fluoroaniline

sodium cyanide

→

4-amino-3-fluorobenzonitrile

용매

N-methylpyrrolidone

반응 조건

후처리

1. 1
   온도The reaction mixture was heated to 190° for 2 hours
2. 2
   온도This mixture was then heated on a steam bath for 2 hours at 60°-70°
3. 3
   추출This aqueous solution was then extracted with four 100-part portions of toluene
4. 4
   세척washed with four 300-part portions of water
5. 5
   건조The toluene solution of the product was dried over sodium sulfate
6. 6
   기타evaporated at a reduced pressure of 50 mm.Hg

실험 절차

6.8 Parts of 4-bromo-2-fluoroaniline were dissolved in 75 parts of N-methylpyrrolidone. This solution was treated with 4.2 parts of cuprous cyanide. The reaction mixture was heated to 190° for 2 hours. The reaction mass was poured into a mixture of 200 parts of ice and 15 parts of sodium cyanide. This mixture was then heated on a steam bath for 2 hours at 60°-70°. This aqueous solution was then extracted with four 100-part portions of toluene. The toluene extracts were combined and washed with four 300-part portions of water followed by 100-parts of saturated aqueous NaCl. The toluene solution of the product was dried over sodium sulfate and evaporated at a reduced pressure of 50 mm.Hg to give 2.6 parts of 4-amino-3-fluorobenzonitrile, m.p. 71°-73°.

출처