تفاعل #67150

ord-d2a66c4f8b3a4b0bab6ec1cc561e84d1

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe solvent was evaporated under a stream of nitrogen
  2. 2
    أخرىthe residue partitioned between ethyl acetate (10 ml) and saturated ammonium chloride (5 ml)
  3. 3
    أخرىThe organic layer was separated by hydrophobic frit
  4. 4
    غسيلwashed with water
  5. 5
    أخرىthe solvent removed in vacuo
  6. 6
    أخرىThe residual solid was purified by Mass Directed Automated Preparative HPLC (Method B)
  7. 7
    أخرىthe solvent was evaporated under a stream of nitrogen

الإجراء التجريبي

Sodium hydroxide (2 ml, 4.00 mmol) was added to a solution of N-[5-[4-(5-{[(2R,6S)-2,6-dimethyl-4-morpholinyl]methyl}-1,3,4-oxadiazol-2-yl)-1-(phenylsulfonyl)-1H-indazol-6-yl]-2-(methyloxy)-3-pyridinyl]-2,4-difluorobenzenesulfonamide (194 mg, 0.212 mmol) in 1,4-dioxane (2 ml). The mixture was stirred at room temperature for 2 h. The solvent was evaporated under a stream of nitrogen and the residue partitioned between ethyl acetate (10 ml) and saturated ammonium chloride (5 ml). The organic layer was separated by hydrophobic frit, washed with water and the solvent removed in vacuo. The residual solid was purified by Mass Directed Automated Preparative HPLC (Method B) and the solvent was evaporated under a stream of nitrogen to give the title compound as a cream coloured solid (10 mg).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08524751B2uspto-grants-2013_09