반응 #68538

ord-0b1c8b07155d420482ef7bede6836449

용매

반응 조건

온도
100°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooled to RT
  2. 2
    농축concentrated in vacuo
  3. 3
    기타Purification by MPLC (DCM/MeOH+1% NH4OH: 100/0 to 90/10)

실험 절차

DMF (0.5 mL) and water (0.1 mL) were added to a pressure vessel containing 8-((6-phenyl-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methylamino)-1,5-naphthyridin-3-ol (50 mg, 135 μmol), sodium 2-chloro-2,2-difluoroacetate (47 mg, 311 μmol), cesium carbonate (62 mg, 190 μmol). The reaction mixture was stirred at 100° C. for 18 h, cooled to RT and concentrated in vacuo. Purification by MPLC (DCM/MeOH+1% NH4OH: 100/0 to 90/10) afforded the title compound (10 mg, 17% yield). MS m/z=420.1 [M+H]+. Calc'd for C21H15F2N7O: 419.40.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08524900B2uspto-grants-2013_09