반응 #67150

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Sodium hydroxide

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

→

title compound

수율 7.7%

N-[5-[4-(5-{[(2R,6S)-2,6-Dimethyl-4-morpholinyl]methyl}-1,3,4-oxadiazol-2-yl)-1H-indazol-6-yl]-2-(methyloxy)-3-pyridinyl]-2,4-difluorobenzenesulfonamide

수율 7.7%

용매

1,4-dioxane

반응 조건

후처리

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

실험 절차

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).

출처