Reaktion #88345

Reaktionsgleichung

Vemurafenib

HCl

ethanol

→

Vemurafenib HCl

Lösungsmittel

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwere added dropwise
2. 2
   SonstigeA clear solution was obtained
3. 3
   Temperaturto cool to RT
4. 4
   workup.STIRRINGstirred overnight
5. 5
   FiltrationThe obtained precipitate was filtered
6. 6
   Waschenwashed with acetone
7. 7
   Sonstigedried at 40° C. under reduced pressure (30 mbar) for approximately 16 h

Vorschrift

Vemurafenib (97.8 g, 199.6 mmol) was suspended in 900 mL acetone and the mixture was warmed to 35° C. While maintaining this temperature, 200 ml of 1.25 M HCl in ethanol (250 mmol HCl, 1.25 equivalents) were added dropwise. A clear solution was obtained. Thereafter, the solution was stirred for another 5 min at 35° C. and then allowed to cool to RT and stirred overnight. The obtained precipitate was filtered, washed with acetone and dried at 40° C. under reduced pressure (30 mbar) for approximately 16 h. Yield: 95.8 g (91%)

Quelle