[N+:1]([C:4]1[CH:5]=[C:6]([CH:12]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:14]=1)[C:7]([N:9]([CH3:11])[CH3:10])=[O:8])([O-])=O>C1COCC1.[Ni]>[NH2:1][C:4]1[CH:5]=[C:6]([CH:12]=[C:13]([C:15]([F:16])([F:17])[F:18])[CH:14]=1)[C:7]([N:9]([CH3:11])[CH3:10])=[O:8]Hydrogenation of (3-nitro-N,N-dimethyl-5-trifluoromethyl-benzamide (12.6 g, 48 mmol) in THF (250 ml) in the presence of Raney-Nickel (3 g), filtration through celite, concentration of the filtrate and crystallization from hexane gives the title compound: m.p.: 154° C.; MS: [M+1]+=233; 1H-NMR (CD3OD): 6.97 (s, 1H), 6.84 (s, 2H), 3.09 (s, 3H), 2.99 (s, 3H).
Wird geladen…