반응 #41532

ord-5739102b7b02496e84958cd0c1d66046

반응 조건

온도
160°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the reaction liquid
  2. 2
    기타The reaction liquid
  3. 3
    세척washed with water and saturated saline in order
  4. 4
    건조dried with anhydrous magnesium sulfate
  5. 5
    기타The solvent was evaporated away under reduced pressure
  6. 6
    기타the resulting residue was purified
  7. 7
    기타through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), ethyl acetate)
  8. 8
    기타to obtain the entitled compound

실험 절차

5.0 mg of sodium hydride was added to a dimethylformamide (0.5 ml) solution of 16 mg of 4-(4-fluoro-phenoxy)-2-methanesulfonyl-6-(pyridin-3-yloxy)-1H-benzimidazole, and then 10.4 mg of [1,2,4]triazole was added to it, and the reaction liquid was stirred overnight at 160° C. The reaction liquid was diluted with ethyl acetate, washed with water and saturated saline in order, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), ethyl acetate) to obtain the entitled compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07728025B2uspto-grants-2010_06