Lithium Hydroxide → HCID 68866177、化合物

反応式

C([O:8][C:9](=[O:35])[CH2:10][CH2:11]/[CH:12]=[CH:13]/[C:14]1[CH:23]=[CH:22][CH:21]=[C:20]([NH:24][S:25]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=2[F:34])(=[O:27])=[O:26])[C:15]=1[C:16]([O:18][CH3:19])=[O:17])C1C=CC=CC=1.[Li+].[OH-]>CO.[OH-].[OH-].[Pd+2]>[F:34][C:29]1[CH:30]=[CH:31][CH:32]=[CH:33][C:28]=1[S:25]([NH:24][C:20]1[C:15]([C:16]([O:18][CH3:19])=[O:17])=[C:14]([CH2:13][CH2:12][CH2:11][CH2:10][C:9]([OH:35])=[O:8])[CH:23]=[CH:22][CH:21]=1)(=[O:27])=[O:26]

参加物

実験手順

A solution of Example 510D (9.84 g, 19.77 mmol) in methanol (150 mL) was added to Pd(OH)2 (1.97 g). The suspension was shaken in a reactor pressurized with 60 psi of H2 at 25° C. for 24 hours, filtered, and concentrated. The concentrate was dissolved in 4:1 methanol/H2O (200 mL), treated with LiOH (1.38 g, 57.66 mmol), stirred for 18 hours, quenched with 1N HCl (100 mL), and concentrated. The remaining solution was extracted with ethyl acetate (2×100 mL). The combined extracts were washed with brine (100 mL), dried (MgSO4), filtered, and concentrated to provide desired product (7.80 g, 96%). MS (ESI(+)) m/e 427 (M+NH4)+, 432 (M+Na)+; MS (ESI(−)) m/e 408 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ 11.97 (br s, 1H), 10.05 (br s, 1H), 7.68 (m, 2H), 7.41 (dd, 1H), 7.31 (t, 2H), 7.15 (d, 1H), 7.02 (d, 1H), 3.66 (s, 3H), 2.53 (m, 2H), 2.17 (m, 2H), 1.44 (m, 4H).