Sodium Sulfate → HCID 58238575、化合物

反応式

[H-].[H-].[H-].[H-].[Li+].[Al+3].[CH:7]([C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([CH:16]([CH3:18])[CH3:17])[C:11]=1[N:19]=[C:20]([C:22]1[CH:23]=[C:24]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=2[O:34][CH3:35])[CH:25]=[CH:26][CH:27]=1)[CH3:21])([CH3:9])[CH3:8].[O-]S([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[CH:7]([C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([CH:16]([CH3:18])[CH3:17])[C:11]=1[NH:19][CH:20]([C:22]1[CH:23]=[C:24]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=2[O:34][CH3:35])[CH:25]=[CH:26][CH:27]=1)[CH3:21])([CH3:8])[CH3:9]

参加物

実験手順

To a suspension of 0.70 g (18.4 mmol) of LiAlH4 in 60 mL of THF, 2.25 g (5.84 mmol) of 39 was added. This reaction mixture was refluxed for 2 hr, and then saturated aqueous Na2SO4 was added. The organic layer was separated, and the aqueous layer was extracted with 2×50 mL of diethyl ether. The combined organic extract was evaporated to dryness, and the product was isolated by flash chromatography on silica gel 60 (40-63 um, eluent: hexanes-diethyl ether from 100:1 to 20:1, vol.) to yield 1.45 g (64%) of Fl.