反应 #1234024
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09000025B2
反应条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 3-Bromo-4-methoxy-benzoic acid ethyl ester (1.61 g, 6.62 mmol) and isooctyl-3-mercaptopropionate (1.73 g, 7.95 mmol) were dissolved in dioxane (26 mL) and the mixture was sparged with N2 (g) for 10 minutes. Diisopropylethyl amine (2.31 mL, 13.25 mmol), Xanthphos (0.1917 g, 0.33 mmol) and tris(dibenzylideneacetone)dipalladium(0) (0.1517 g, 0.166 mmol) were added and the mixture was sparged with N2 (g) for 5 minutes. The reaction was then heated to 90° C. for 2 hours after which time it was filtered to remove solid impurities. The mixture was concentrated and the residue was purified on silica gel (0-40% EtOAc in hexanes) to give the title compound. the mixture was sparged with N2 (g) for 10 minutes the mixture was sparged with N2 (g) for 5 minutes was filtered to remove solid impurities The mixture was concentrated the residue was purified on silica gel (0-40% EtOAc in hexanes)
来源 ID: ord-ec88ccc5db564be69341524009f9268d