HRID47009

反应详情

EQUATION

反应方程式

HRID 47009 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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°.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated to 190° for 2 hours
  2. temperatureThis mixture was then heated on a steam bath for 2 hours at 60°-70°
  3. extractionThis aqueous solution was then extracted with four 100-part portions of toluene
  4. washwashed with four 300-part portions of water
  5. dry with materialThe toluene solution of the product was dried over sodium sulfate
  6. customevaporated at a reduced pressure of 50 mm.Hg