HRID602589

反应详情

EQUATION

反应方程式

HRID 602589 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

step 3—A solution of 3-bromo-5-methoxy-benzaldehyde (1 mmol) in DMF (2 mL) is added to a round bottomed flask containing Zn(CN)2 (0.7 equivalents), Pd(PPh3)4(0) (0.2 equivalents) in DMF (15 mL). The reaction is stirred at 90° C. under an atmosphere of argon for 48 h. The reaction mixture is cooled and evaporated to dryness. The crude residue is dissolved in EtOAc, washed with brine solution, dried (MgSO4) and evaporated. The crude product is purified by SiO2 chromatography to afford 3-formyl-5-methoxy-benzonitrile.

WORKUP

后处理

  1. temperatureThe reaction mixture is cooled
  2. customevaporated to dryness
  3. dissolutionThe crude residue is dissolved in EtOAc
  4. washwashed with brine solution
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customThe crude product is purified by SiO2 chromatography