Réaction #41263

ord-8ec567fe6a224eab86469cfeafb1c7e5

Conditions de réaction

Température
40°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autrewas prepared
  2. 2
    Températuremaintained for 1.5 hrs
  3. 3
    TempératureIt was further heated to about 70° C
  4. 4
    FiltrationThe suspension was then filtered
  5. 5
    Températurethe supernatant cooled to ambient temperatures naturally in the water bath

Mode opératoire

2-{4′-[(3aR,6aR)-5-Methylhexahydropyrrolo[3,4-b]pyrrol-1(2H)-yl]-1,1′-biphenyl-4-yl}pyridazin-3(2H)-one tartrate (Form A) was suspended in 1 mL of solution mixture, which was prepared by mixing 3.0 mL of dichloromethane with 1.5 mL of 20% water (in methanol). The suspension was vortexed and heated in a shaking water bath to about 40° C. and maintained for 1.5 hrs. It was further heated to about 70° C. The suspension was then filtered. The water bath was turned off, and the supernatant cooled to ambient temperatures naturally in the water bath. Single crystals were offered.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07728031B2uspto-grants-2010_06