反応 #43330

ord-9ed94748395b45b697f76c4f2d4a5178

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度under reflux
  2. 2
    洗浄by washing with saturated aqueous sodium hydrogencarbonate solution and saturated brine
  3. 3
    乾燥drying over anhydrous sodium sulfate
  4. 4
    濃縮Concentrating the solvent under reduced pressure
  5. 5
    workup.DISTILLATIONthe resulting residue was distilled under reduced pressure (63° C., 8 mmHg)

実験手順

A mixture of 2,5-dichloropyridine (10.0 g), potassium vinyltrifluoroborate (10.86 g), dichloromethane complex (2.5 g) of dichloro-1,1′-bis(diphenylphosphino)-ferrocene palladium (II), triethylamine (14.13 mL) and ethanol (150 mL) was stirred overnight under reflux. After cooling the system to room temperature, ethyl acetate was added, followed by washing with saturated aqueous sodium hydrogencarbonate solution and saturated brine and drying over anhydrous sodium sulfate. Concentrating the solvent under reduced pressure, the resulting residue was distilled under reduced pressure (63° C., 8 mmHg) to provide the title compound (6.50 g, 69%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07732456B2uspto-grants-2010_06