Reaktion #171180

ord-769ce9bd32174e8c9ea7e68844bffc18

Reaktionsbedingungen

Temperatur
55°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeat room temperature
  2. 2
    SonstigeThe reaction mixture was then quenched
  3. 3
    SonstigeThe solvents were evaporated under reduced pressure
  4. 4
    SonstigeThe residue thus obtained
  5. 5
    SonstigeThe organic layer was separated
  6. 6
    Waschenwashed with water and brine solution
  7. 7
    Trocknendried over anhydrous sodium sulphate
  8. 8
    EinengenThe solvent was concentrated under reduced pressure

Vorschrift

Perchloric acid (0.2 mL) was added to a solution of the compound obtained from step l above (0.3 g) in acetonitrile (4 mL) and water (0.2 mL) at room temperature. The reaction mixture was heated to 55° C. for 30 minutes. The reaction mixture was then quenched using sodium bicarbonate solution. The solvents were evaporated under reduced pressure. The residue thus obtained was taken up in ethyl acetate and water. The organic layer was separated and washed with water and brine solution and dried over anhydrous sodium sulphate. The solvent was concentrated under reduced pressure to yield the title compound (0.25 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846910B2uspto-grants-2014_09