反应 #1600800
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06673797B1
反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 1-benzenesulfonylamino-2-iodo-4-methanesulfonylbenzene (256 mg) in 1,4-dioxane (6 ml), 2-ethynyltetrahydrofuran (169 mg), bistriphenylphosphine palladium dichloride (21 mg), cuprous iodide (11 mg) and triethylamine (89 mg) were added successively and the mixture was stirred in a sealed tube at 60° C. for 3 hours. After cooling, the reaction solution was poured into water, extracted with dichloromethane, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The resulting residue was separated using silica gel preparative thin-layer chromatography (hexane:ethyl acetate=1:1) to obtain 218 mg of the desired product in a white amorphous form. After cooling extracted with dichloromethane dried over anhydrous magnesium sulfate filtered concentrated under reduced pressure The resulting residue was separated
来源 ID: ord-69ea4f2f131c4410be81dd751da3a87c