[F:1][C:2]([F:12])([F:11])[C:3]1[N:4]=[C:5]([C:8](=[NH:10])[NH2:9])[S:6][CH:7]=1.CC[O-].[Na+].O=[C:18]([C:25]1[S:26][CH:27]=[C:28]([C:30]([F:33])([F:32])[F:31])[N:29]=1)[CH2:19][C:20](OCC)=[O:21]>C(O)C>[F:12][C:2]([F:1])([F:11])[C:3]1[N:4]=[C:5]([C:8]2[N:9]=[C:20]([OH:21])[CH:19]=[C:18]([C:25]3[S:26][CH:27]=[C:28]([C:30]([F:32])([F:33])[F:31])[N:29]=3)[N:10]=2)[S:6][CH:7]=1To a solution of compound 27 (0.43 mmol) and NaOEt (2.15 mmol) in ethanol (2 mL) was added compound 28 (0.43 mmol). The reaction mixture was stirred at 100° C. overnight. The solvent was evaporated and water and AcOEt were added. The aqueous layer was acidified to pH˜4-5 by addition of 2.5M HCl. The organic layer was dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by silica gel chromatography (eluent: DCM/MeOH 0 to 5%) to give compound 29 as a beige solid in 11% yield. MS (ESI, EI−): m/z=396.91 (MH−).
読み込み中…
