Reaktion #491345

ord-bd178b056ab04afabae2daf7c2d61114

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added
  2. 2
    Sonstigefollowed by the removal of the solvent under reduced pressure
  3. 3
    SonstigeThe resulting dry
  4. 4
    Sonstigewas purified by silica gel column chromatography
  5. 5
    Wascheneluting with hexane/EtOAc (60:40

Vorschrift

Compound I (2.325 mg, 8.80 mmol), 2-aminopyridine (911 mg, 9.68 mmol), tBuOK (1.481 g, 13.20 mmol), (±)-BINAP (219 mg, 0.35 mmol) and Pd2(dba)3 (201 mg, 0.22 mmol) were stirred in toluene (35 mL) at 90° C. under Ar(g) for 17 h. The reaction mixture was then diluted with CH2Cl2 (20 mL) and silica was added followed by the removal of the solvent under reduced pressure. The resulting dry loaded material was purified by silica gel column chromatography eluting with hexane/EtOAc (60:40 then 50:50) to furnish II as a yellow oil (1.773 g, 73%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08748458B2uspto-grants-2014_06