[CH3:1][N:2]1[C:6]([C:7]([NH2:9])=[O:8])=[C:5]([N+:10]([O-])=O)[C:4]([CH2:13][CH2:14][CH3:15])=[N:3]1.[H][H]>[Pd].C(OCC)(=O)C>[NH2:10][C:5]1[C:4]([CH2:13][CH2:14][CH3:15])=[N:3][N:2]([CH3:1])[C:6]=1[C:7]([NH2:9])=[O:8]A stirred suspension of 1-methyl4-nitro-3-n-propylpyrazole-5-carboxamide (EP-A-0463756; 237.7 g, 1.12 mol) and 5% palladium on charcoal (47.5 g) in ethyl acetate (2.02 l) was hydrogenated at 344.7 kPa (50 psi) and 50° C. for 4 hours, when the uptake of hydrogen was complete. The cool reaction mixture was filtered, then the filter pad washed with ethyl acetate, the combined filtrate and washings thus furnishing an ethyl acetate solution of the title compound (EP-A-0463756) which was of sufficient purity to use directly in the next stage of the reaction sequence (see Preparation 4).
Wird geladen…
