反应 #3302154
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08013186B2
反应条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1-Fluoro-4-iodobenzene (30 g, 135 mmol) and 2-bromo2,2-difluoroacetic acid ethyl ester (29 g, 142.9 mmol) were dissolved in DMF (100 ml) and Cu (21.5 g, 71.2 mmol) was added. The reaction mixture was heated at 90° C. for 18 h. Ethyl acetate (100 ml) was added and the reaction mixture was quenched with a solution of potassium dihydrogen phosphate (20 g) in water (200 ml). The resultant solution was stirred for 30 min, filtered and was washed with ethyl acetate. The organic layer was separated, washed with water and brine. The organic layer was dried over MgSO4, filtered, and concentrated to give 2,2-difluoro-2-(4-fluorophenyl)acetic acid ethyl ester (26.5 g) as a yellow liquid. the reaction mixture was quenched with a solution of potassium dihydrogen phosphate (20 g) in water (200 ml) filtered was washed with ethyl acetate The organic layer was separated washed with water and brine The organic layer was dried over MgSO4 filtered concentrated
来源 ID: ord-c52f25377984433a8144ca56a9cb0e6c