반응 #169233

ord-c0f719562b684df5a38308d82960f514

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.WAIThydrogenation pursued for an additional 8 hours
  2. 2
    여과The reaction mixture was then filtered
  3. 3
    농축concentrated under reduced pressure

실험 절차

To a solution of 4-[3-cyclohexylethynyl-6-(4-hydroxy-phenyl)-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridine-4-carbonyl]-piperazine-1-carboxylic acid tert-butyl ester (0.34 g, 0.56 mmol) in methanol (15 ml) was added Pd/C (10%, 12 mg, 0.01 mmol). The reaction mixture was hydrogenated at 4 bar for 18 h, Pd/C (10%, 12 mg, 0.01 mmol) was added and hydrogenation pursued for an additional 8 hours. The reaction mixture was then filtered and concentrated under reduced pressure to yield the title compound (0.33 g, 95%) as a grey solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08846712B2uspto-grants-2014_09