반응 #68417

ord-44e6376359eb4a4b9595311267a84bdd

반응 조건

온도
90°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction was then cooled to room temperature
  2. 2
    세척washed with brine
  3. 3
    건조dried over Na2SO4
  4. 4
    농축concentrated in vacuo
  5. 5
    기타The residue was purified by chromatography on silica gel (0→100% EtOAc-hexanes)

실험 절차

General Procedure W. A mixture of 1-benzyl-3-(3,4-difluorobenzylcarbamoyl)-2-isopropyl-1H-indol-6-yl trifluoromethanesulfonate (Compound 160, 50 mg, 0.088 mmol), pyridin-4-ylboronic acid (22 mg, 0.18 mmol), Pd(PPh3)4 (5.0 mg, 0.0043 mmol), K2CO3 (61 mg, 0.44 mmol), and LiCl (19 mg, 0.44 mmol) in toluene (3 ml), MeOH (1 ml), and H2O (0.5 ml) was heated at 90° C. for 16 h. The reaction was then cooled to room temperature, diluted with EtOAc, washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by chromatography on silica gel (0→100% EtOAc-hexanes) to yield the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08524917B2uspto-grants-2013_09