[N+:1]([C:4]1[CH:18]=[C:17]([N+:19]([O-])=O)[CH:16]=[CH:15][C:5]=1[O:6][CH2:7][CH:8]1[CH2:12][O:11][C:10]([CH3:14])([CH3:13])[O:9]1)([O-])=O.[H][H]>[Pd].CO>[NH2:1][C:4]1[CH:18]=[C:17]([NH2:19])[CH:16]=[CH:15][C:5]=1[O:6][CH2:7][CH:8]1[CH2:12][O:11][C:10]([CH3:13])([CH3:14])[O:9]1215 ml of methanol are introduced into a 0.7 l autoclave, 85.3 g (0.3 mole) of 4-(2,4-dinitrophenoxymethyl)-2,2-dimethyl-1,3-dioxolane (step a) are dissolved therein and 0.6 g of palladium on active carbon 10% (Degussa) is added. After the autoclave has been closed and blanketed with nitrogen, hydrogenation is carried out under a pressure of 4 bar and at a temperature of 35 to 40° C. until no more hydrogen is taken up. 1.3 g of active carbon is added under nitrogen to the warm solution and the catalyst is filtered off. 42 g of 70% sulfuric acid are added dropwise to the solution while cooling with ice at 5° C. The product precipitated is filtered off under suction, washed with methanol and dried.
Wird geladen…
