Reaktion #88343

ord-9a7332a9a26743079d78e7b332115661

Reagenzien

Keine

Lösungsmittel

Reaktionsbedingungen

Temperatur
35°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwere added dropwise
  2. 2
    SonstigeA clear solution was obtained
  3. 3
    Temperaturto cool to RT
  4. 4
    FiltrationThe obtained precipitate was filtered
  5. 5
    Waschenwashed with acetone
  6. 6
    Sonstigedried under ambient conditions (RT, atmospheric pressure) for approximately 20 h

Vorschrift

Vemurafenib (Form 2, 0.5 g, 1.02 mmol) was suspended in 5 mL acetone and the mixture was warmed to 35° C. While maintaining this temperature, 0.8 ml of 1.25 M HCl in ethanol (approximately 1 equivalent) were added dropwise. A clear solution was obtained. Thereafter, the solution was allowed to cool to RT and stirred overnight. The obtained precipitate was filtered, washed with acetone and dried under ambient conditions (RT, atmospheric pressure) for approximately 20 h. Yield: 0.49 g (91%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09440971B2uspto-grants-2016_09