반응 #41263

ord-8ec567fe6a224eab86469cfeafb1c7e5

반응 조건

온도
40°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타was prepared
  2. 2
    온도maintained for 1.5 hrs
  3. 3
    온도It was further heated to about 70° C
  4. 4
    여과The suspension was then filtered
  5. 5
    온도the supernatant cooled to ambient temperatures naturally in the water bath

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07728031B2uspto-grants-2010_06