[F:1][C:2]1[C:7]([F:8])=[C:6]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:4][C:3]=1[CH2:12]C(O)=O.FC1C(F)=CC=C([N+]([O-])=O)C=1CC(O)=O.C(=O)([O-])[O-].[K+].[K+].FC1C(F)=CC=C([N+]([O-])=O)C=1C>CN(C)C=O>[F:1][C:2]1[C:7]([F:8])=[C:6]([N+:9]([O-:11])=[O:10])[CH:5]=[CH:4][C:3]=1[CH3:12]The mixture of 2,3-difluoro-4-nitrophenylacetic acid and 2,3-difluoro-6-nitrophenylacetic acid from D16 (13.5 g) was dissolved in dimethylformamide (100 ml) and potassium carbonate (8.5 g) added. After stirring at 50° C. for 30 min the cooled solution was partitioned between aqueous hydrochloric acid and hexane. Drying (MgSO4), evaporation, and chromatography (0-5% ethyl acetate in hexane, 70 g silica column) gave 3.2 g of a 3:1 mixture of the title compound and 2,3-difluoro-6-nitrotoluene.
読み込み中…
