反应 #1990771
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07687502B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 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. The reaction solution was filtered chloroform was added to the filtrate the mixture was washed with a saturated aqueous solution of sodium hydrogen carbonate The organic layer was dried concentrated the resulting residue was purified by a silica gel column chromatography (hexane:ethyl acetate=2:1)
来源 ID: ord-5ebaa3e9af374c4c97da47c985b54541