HRID343925

反应详情

EQUATION

反应方程式

HRID 343925 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A stirred mixture of 4-bromo-2-fluorobenzaldehyde (39 g, 192 mmol) and cuprous cyanide (18.9 g, 211 mmol) in dimethylformamide (100 ml) was heated to 150° C. for 12 hours under nitrogen atmosphere. The dark solution was cooled and a solution of ferric chloride (34 g, 211 mmol) in hydrochloric acid (2M, 100 ml) was added, followed by water (100 ml). Solid crystallised from the mixture and was filtered, washed with water and dried at 40° C. in vacuo. Recrystallisation from cyclohexane (500 ml) gave 4-cyano-2-fluorobenzaldehyde (m.p. 79° C.) as yellow needles.

WORKUP

后处理

  1. temperatureThe dark solution was cooled
  2. customSolid crystallised from the mixture
  3. filtrationwas filtered
  4. washwashed with water
  5. customdried at 40° C. in vacuo
  6. customRecrystallisation from cyclohexane (500 ml)