反应详情

Under argon atmosphere, a mixture comprising 1.0 g trans-4-(benzyloxycarbonylamino)cyclohexanecarbonyl chloride, 1.92 g of tributylphenyltin, 61 mg of dichlorobis(triphenylphosphine)palladium and 10 mL of dioxane was stirred at 110° C. for 12 hours. After cooling, the reaction mixture was concentrated by a centrifugal concentrator, and then, the residue was dissolved in tetrahydrofuran and evaporated to dryness with 5 g of silica gel. The resulting residue was purified by silica gel flash chromatography (solvent: ethyl acetate-hexane (1:2) to (1:1) to obtain 883 mg of N-benzyloxycarbonyl-trans-4-benzoylcylohexylamine.

1. temperatureAfter cooling
2. concentrationthe reaction mixture was concentrated by a centrifugal concentrator
3. dissolutionthe residue was dissolved in tetrahydrofuran
4. customevaporated to dryness with 5 g of silica gel
5. customThe resulting residue was purified by silica gel flash chromatography (solvent