[C:1]([OH:9])(=[O:8])[C:2]([CH2:4][C:5]([OH:7])=[O:6])=[CH2:3].BrBr.C(=O)([O-])O.[Na+:16].C(=O)([O-])[O-].[Na+].[Na+]>O>[O:6]=[C:5]1[O:7][CH2:3][C:2]([C:1]([O-:9])=[O:8])=[CH:4]1.[Na+:16]To a solution of itaconic acid (26.0 g) in water (35 ml) was added dropwise bromine (10.3 ml) at room temperature while keeping a temperature of the reaction solution below 45° C., and then the mixture was stirred at 30° C. for 15 minutes. To this reaction solution was added portionwise sodium hydrogen carbonate (33.6 g), and then the mixture was heated to 55° C. To this reaction solution was added dropwise a solution of sodium carbonate (10.6 g) in water (15 ml), and then the mixture was stirred for 20 minutes. This reaction solution was iced, and stirred for 1 hour. The precipitated solid was collected by filtration, washed with cold water and ethanol, and then dried under reduced pressure to give the titled compound (16.8 g).
Wird geladen…
