C([O-])(=O)C.[Na+].Cl.[NH2:7][OH:8].[F:9][C:10]1[CH:15]=[CH:14][C:13]([CH2:16][C:17]([C:19]2[CH:24]=[CH:23][N:22]=[CH:21][CH:20]=2)=O)=[CH:12][CH:11]=1>CO>[F:9][C:10]1[CH:15]=[CH:14][C:13]([CH2:16][C:17]([C:19]2[CH:24]=[CH:23][N:22]=[CH:21][CH:20]=2)=[N:7][OH:8])=[CH:12][CH:11]=1Sodium acetate (36.1 g; 0.44 mol) and hydroxylamine hydrochloride (22.0 g; 0.32 mol) were introduced into a suspension of a2 (21.5 g; 0.1 mol) in 50% strength methanol (350 ml). The reaction mixture was stirred under reflux for 1 h. When the clear solution was cooled in an ice bath, a3 was obtained as a beige precipitate which was filtered off, washed with H2O and dried under reduced pressure over P2O5.
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