反应详情

1,2-Difluoro-3-iodobenzene (1.70 g; 7.08 mmol), 2.17 g (21.2 mmol) of sodium methanesulfonate and 4.03 g (21.2 mmol) of copper iodide were heated with stirring at 111° C. for 20 hours in 50 ml of N,N-dimethylacetamide. The reaction solution was filtered, chloroform was added to the filtrate and the mixture was washed with a saturated aqueous solution of sodium hydrogen carbonate. The organic layer was dried and concentrated and the resulting residue was purified by a silica gel column chromatography (hexane:ethyl acetate=2:1) to give 987 mg (yield: 72%) of 1,2-difluoro-3-methanesulfonylbenzene as a colorless transparent solution.

1. filtrationThe reaction solution was filtered
2. additionchloroform was added to the filtrate
3. washthe mixture was washed with a saturated aqueous solution of sodium hydrogen carbonate
4. customThe organic layer was dried
5. concentrationconcentrated
6. customthe resulting residue was purified by a silica gel column chromatography (hexane:ethyl acetate=2:1)