[O:1]=[C:2]1[N:6]([CH2:7][CH2:8][O:9][C:10]2[CH:27]=[CH:26][C:13]([CH:14]=[C:15]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[C:16]([O:18][CH2:19][CH3:20])=[O:17])=[CH:12][CH:11]=2)[C:5]2[CH:28]=[CH:29][CH:30]=[CH:31][C:4]=2[O:3]1>O1CCOCC1.[Pd]>[O:1]=[C:2]1[N:6]([CH2:7][CH2:8][O:9][C:10]2[CH:11]=[CH:12][C:13]([CH2:14][CH:15]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[C:16]([O:18][CH2:19][CH3:20])=[O:17])=[CH:26][CH:27]=2)[C:5]2[CH:28]=[CH:29][CH:30]=[CH:31][C:4]=2[O:3]1Dissolve the compound obtained in Example 1 (6.7 g) in a dioxane/absolute ethanol mixture (100 ml/20 ml) and add palladium-on-carbon (0.5 g). Stir magnetically at ambient temperature under a hydrogen atmosphere for 76 hours. Remove the palladium-on-carbon by filtration and remove the mixture of solvents by evaporation under reduced pressure. Crystallise the resulting oil by trituration in isopropyl ether. Recrystallise the resulting precipitate from a 9/1 cyclohexane/toluene mixture.
Wird geladen…