[C:1]1([C:7]2[C:8]3[N:9]([CH:13]=[CH:14][N:15]=3)[CH:10]=[CH:11][CH:12]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(=O)(=O)(O)O.[N+:21]([O-])([OH:23])=[O:22].C(=O)([O-])[O-].[K+].[K+]>O>[N+:21]([C:4]1[CH:3]=[CH:2][C:1]([C:7]2[C:8]3[N:9]([CH:13]=[CH:14][N:15]=3)[CH:10]=[CH:11][CH:12]=2)=[CH:6][CH:5]=1)([O-:23])=[O:22]Add 20 g (0.10 mole) of the product from Example 4 slowly to 150 ml of concentrated sulfuric acid at -15° C. Add 7 ml of concentrated nitric acid slowly, maintaining the temperature -10° C. Stir at -10° C. for 30 minutes. Pour onto 500 g of ice. Add 2 L of water and neutralize with potassium carbonate. Extract with three 500 ml portions of methylene chloride. Combine the extracts, dry over magnesium sulfate, treat with charcoal and remove the solvent in vacuo. The residue is crystallized from ether to provide the title compound.
Wird geladen…
