[OH-].[Na+].[N+:3]([CH2:6][C:7]([C:9]1C=CC=[CH:11][CH:10]=1)=O)([O-:5])=[O:4].[Cl:15][C:16]1[C:17]([CH:26]=O)=[N:18][CH:19]=[C:20]([C:22]([F:25])([F:24])[F:23])[CH:21]=1.[C:28]([OH:31])(=O)[CH3:29].[CH2:32](O)C>O>[Cl:15][C:16]1[C:17]([CH:26]=[CH:32][C:28]([C:29]2[CH:11]=[CH:10][CH:9]=[CH:7][C:6]=2[N+:3]([O-:5])=[O:4])=[O:31])=[N:18][CH:19]=[C:20]([C:22]([F:23])([F:24])[F:25])[CH:21]=1Sodium hydroxide (0.55 g) was dissolved in water (5 ml) and the resulting solution was diluted with ethanol (3 ml). 2-Nitroacetophenone (1.8 g) was added at 20° C., and the solution was stirred for 5 minutes. 3-Chloro-5-(trifluoromethyl)pyridine-2-carboxaldehyde (2.25 g) was added and stirring was continued for 16 hours. The solution was acidified with acetic acid, the organic layer separated, dried over magnesium sulfate, filtered and evaporated to give a brown oil. Silica gel column chromatography, followed by recrystallisation (petrol) afforded the title compound, 88-9° C.
Wird geladen…