HRID423321

反应详情

EQUATION

反应方程式

HRID 423321 的结构方程式

PROCEDURE

实验过程

To a solution of 4-bromo-3-trifluoromethylbenzonitrile (1.25 g, 5.0 mmol) and isobutylzinc bromide (25 mmol) in THF (50 mL, 25 mmol) under argon was added 1,1′-bis(diphenylphosphino)ferrocenedichloro palladium(II) dichloromethane complex (612 mg, 0.75 mmol) and the reaction heated at reflux for 5 h. The mixture was concentrated in vacuo and the residue partitioned between ethyl acetate (80 mL) and water (80 mL). A solid formed and was filtered off and discarded. The organic layer was washed with water (80 mL) before it was dried (phase separator) and concentrated in vacuo to give the crude title compound as a black oil. This was used directly in the next step (1.35 g).

WORKUP

后处理

  1. temperaturethe reaction heated
  2. temperatureat reflux for 5 h
  3. concentrationThe mixture was concentrated in vacuo
  4. customthe residue partitioned between ethyl acetate (80 mL) and water (80 mL)
  5. customA solid formed
  6. filtrationwas filtered off
  7. washThe organic layer was washed with water (80 mL) before it
  8. customwas dried (phase separator)
  9. concentrationconcentrated in vacuo