Reaktion #162630

ord-1bce316c12b245bfb48278a76c850844

Lösungsmittel

Reaktionsbedingungen

Temperatur
140°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto give a yellow suspension
  2. 2
    EinengenThe mixture was concentrated
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in dichloromethane
  4. 4
    Waschenwashed
  5. 5
    TrocknenThe organic phase was dried over MgSO4
  6. 6
    Filtrationfiltered
  7. 7
    Einengenconcentrated

Vorschrift

In a 2-5 mL microwave vial was placed 8-(6-chloro-2-(4-nitrophenyl)pyrimidin-4-yl)-3-oxa-8-azabicyclo[3.2.1]octane (36, 200 mg, 0.577 mmol) in iPrNH2 (5 mL) to give a yellow suspension. The reaction was heated under microwave irradiation at 140° C. for 3×45 min. The mixture was concentrated. The residue was dissolved in dichloromethane and washed with sat NaHCO3. The organic phase was dried over MgSO4, filtered and concentrated to give the title compound (208 mg, 98%) as a yellow foam. HRMS: For [M+H]+ mass error=0.1 mDa or 0.23 ppm.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08835429B2uspto-grants-2014_09