HRID1744517

反应详情

EQUATION

反应方程式

HRID 1744517 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3′-Bromo-4′-isobutylacetophenone (182 g) and copper cyanide (95.7 g) were stirred in dimethylformamide (520 ml) at 140° C. for 7 h. The reaction mixture was cooled to room temperature and the solid was filtered off. To the filtrate was added water and the mixture was extracted with toluene. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate, after which the solvent was evaporated under reduced pressure. The residue was recrystallized from n-hexane to give 3′-cyano-4′-isobutylacetophenone (70 g), melting point: 71–72° C.

WORKUP

后处理

  1. filtrationthe solid was filtered off
  2. additionTo the filtrate was added water
  3. extractionthe mixture was extracted with toluene
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customafter which the solvent was evaporated under reduced pressure
  7. customThe residue was recrystallized from n-hexane