Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([Cl:11])[N:5]=[C:4](C)[C:3]=1[C:13]([OH:15])=[O:14].[CH2:16](N(CC)CC)[CH3:17].[NH3:23].O1CCOCC1>ClCCl>[CH2:16]([O:15][C:13]([C:3]1[CH:4]=[N:5][C:6]([Cl:11])=[C:7]([N+:8]([O-:10])=[O:9])[C:2]=1[NH2:23])=[O:14])[CH3:17]To a solution of 4,6-Dichloro-2-methyl-5-nitro-pyridine-3-carboxylic acid (15 g, 56.6 mmol) and triethylamine (7.9 mL, 57.3 mmol) in dichloromethane (84 mL) at 0° C. was added dropwise ammonia solution in dioxane (0.5 M, 113 mL, 56.5 mmol). The mixture was then stirred overnight. Removal of the solvent followed by column chromatography gave 9 as a yellow crystalline solid. (7.3 g). 1H-NMR δ: 1.32 (t, J=7.1 Hz, 3H), 4.33 (q, J=7.1 Hz, 2H), 8.06 (s, br, 2H), 8.62 (s, 1H).
Wird geladen…
