反应详情

5-{4-[(5S)-5-(aminomethyl)-2-oxo-1,3-oxazolidin-3-yl]-2,6-difluorophenyl}piperidin-2-one (0.1 g, 0.31 mmol) (prepared by the route described in Example 1, substituting N-{[(5S)-3-(3,5-difluoro-4-iodophenyl)-2-oxo-1,3-oxazolidin-5-yl]methyl}acetamide) is dissolved in MeOH (2 mL). To this mixture is added Et3N (0.125 ml, 0.9 mmol) and N′-[(1E)-2,2-dichloroethylidene]-4-methylbenzenesulfonohydrazide (0.17 g, 0.6 mmol)(Prepared in Example 26 step 1). The reaction is stirred at 0° C. to RT for 16 hours. The mixture was concentrated to dryness, reconstituted in CH2Cl2 (125 mL) and extracted with H2O. The organic layer was dried (MgSO4), loaded onto a SIM and purified on a Biotage 12M column to yield (0.033 g, 30%). 1H-NMR (DMSO) δ: 8.17, 7.77, 7.61, 7.25, 5.16, 4.83, 4.21, 3.87, 3.28, 3.18, 2.29, 1.86

1. concentrationThe mixture was concentrated to dryness
2. extractionextracted with H2O
3. dry with materialThe organic layer was dried (MgSO4)
4. custompurified on a Biotage 12M column
5. customto yield (0.033 g, 30%)