Reaktion #621031

ord-0e0c5a24b14b4597b9ea8e66db88e5b5

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenconcentrated under vacuum
  2. 2
    workup.ADDITIONThe resulting residue was treated with H2O (4 mL)
  3. 3
    Extraktionextracted with DCM (8 mL)
  4. 4
    SonstigeThe organic layer was dried through a phase separator
  5. 5
    Einengenconcentrated under vacuum
  6. 6
    Sonstigepurified by preparatory HPLC (without TFA)

Vorschrift

To a solution of 3-biphenylol (0.0574 g, 0.337 mmol) in acetonitrile (4 mL) was added 1,3-dibromopropane (0.340 mL, 3.35 mmol) followed by Cs2CO3 (0.172 g, 0.529 mmol). The reaction mixture was stirred for 24 h and then concentrated under vacuum. The resulting residue was treated with H2O (4 mL) and extracted with DCM (8 mL). The organic layer was dried through a phase separator and concentrated under vacuum. The residue was taken up in DMSO and purified by preparatory HPLC (without TFA) to give the title compound (0.0568 g, 57.8%). EI-MS Rt (2.59 min).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08853404B2uspto-grants-2014_10