Reaktion #717554

ord-b9a79797034d4efdbd42f595d1b0a9a5

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstige(about 20 h)
  2. 2
    Sonstigeis then reduced to about 50° C.
  3. 3
    TemperaturThe resulting mixture is maintained
  4. 4
    Temperaturcooled to room temperature
  5. 5
    SonstigeThe phases are separated
  6. 6
    workup.ADDITIONthe organic phase is treated with decolourising carbon
  7. 7
    EinengenThe organic phase is then concentrated under vacuum
  8. 8
    Sonstigeto obtain a sandy solid
  9. 9
    Sonstigewhich is isolated by filtration (at 0-5° C.)
  10. 10
    Sonstigedried under vacuum at 40° C. for 8 h (about 15 g)

Vorschrift

Acetic anhydride (70 g) is added to a suspension of Abiraterone (16 g) in ethyl acetate (48 mL) The mixture is heated to 70° C. until the reaction is complete (about 20 h); the temperature is then reduced to about 50° C. and methanol (28 mL) is added. The resulting mixture is maintained under stirring for 2 h, cooled to room temperature, and ethyl acetate (110 mL) and an aqueous solution of sodium carbonate (450 mL) are added. The phases are separated and the organic phase is treated with decolourising carbon. The organic phase is then concentrated under vacuum and the concentrate is taken up with acetonitrile (about 80 mL) to obtain a sandy solid, which is isolated by filtration (at 0-5° C.) and dried under vacuum at 40° C. for 8 h (about 15 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09315541B2uspto-grants-2016_04