반응 #43330

ord-9ed94748395b45b697f76c4f2d4a5178

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도under reflux
  2. 2
    세척by washing with saturated aqueous sodium hydrogencarbonate solution and saturated brine
  3. 3
    건조drying over anhydrous sodium sulfate
  4. 4
    농축Concentrating the solvent under reduced pressure
  5. 5
    workup.DISTILLATIONthe resulting residue was distilled under reduced pressure (63° C., 8 mmHg)

실험 절차

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07732456B2uspto-grants-2010_06