HRID647327

反应详情

EQUATION

反应方程式

HRID 647327 的结构方程式

PROCEDURE

实验过程

To a slurry of 39 g of aluminum chloride and 120 ml of 1,3-difluorobenzene was added dropwise, with stirring, 30 g of N-formylisonipecotic acid chloride. The reaction mixture was stirred under reflux for two hrs and poured into 1 l of ice-water. The mixture was extracted with 4 350-ml portions of chloroform. The combined organic extracts were washed with 2 300-ml portions of water, dried, filtered and evaporated. Trituration with petroleum ether and washing with ether at 0°, yielded 14 g (32.3%) of product, mp, 75°.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred
  2. temperatureunder reflux for two hrs
  3. extractionThe mixture was extracted with 4 350-ml portions of chloroform
  4. washThe combined organic extracts were washed with 2 300-ml portions of water
  5. customdried
  6. filtrationfiltered
  7. customevaporated
  8. washTrituration with petroleum ether and washing with ether at 0°