[CH3:1][S:2][C:3]1[CH:4]=[C:5]([C:10]([C:12]2[S:13][CH:14]=[CH:15][N:16]=2)=[O:11])[CH:6]=[C:7]([F:9])[CH:8]=1.C1C=C([O:23]O)C(C(O)=O)=C(C(O)=O)C=1.C([O-])(O)=O.[Na+]>CO.C(Cl)Cl>[CH3:1][S:2]([C:3]1[CH:4]=[C:5]([C:10]([C:12]2[S:13][CH:14]=[CH:15][N:16]=2)=[O:11])[CH:6]=[C:7]([F:9])[CH:8]=1)=[O:23]To a solution of sulfide from Step 1 (0.76 g, 2.99 mmol) in MeOH (1.5 mL) and CH2Cl2 (6 mL) at 0° C. was added the magnesium salt of monoperoxyphthalic acid (1.11 g, 1.80 mmol). The mixture was stirred at 0° C. for 1.25 h and then sat. aqueous NaHCO3 was added. The layers were separated and the aqueous phase was extracted with CH2Cl2. The combined organic layers were washed with H2O and dried over anhydrous MgSO4. Evaporation of the solvent and chromatography using toluene:EtOAc (25:75) gave 0.70 g of the title compound.
読み込み中…
