反应详情

To toluene 3.0 mL suspension of tert-butyl 2-amino-4-phenylbenzoate 0.20 g, 2-dicyclohexylphosphino-2′,4′,6′-triisopropylbiphenyl 17 mg, tris(dibenzylideneacetone)dipalladium(0) 7 mg, palladium acetate 2 mg and cesium carbonate 0.48 g was added tert-butyl 5-bromoindol-1-carboxylate 0.55 g, and it was heated and refluxed for 8 hours. After the reaction mixture was cooled to room temperature, insoluble matter was filtrated, and ethyl acetate and 10% citric acid aqueous solution were added to it. The organic layer was separated and collected,dried over anhydrous magnesium sulfate after washing with saturated sodium chloride aqueous solution, and the solvent was removed under reduced pressure. The obtained residue was refined by silica gel column chromatography [Trikonex company, Flash Tube 2008, eluent; hexane:ethyl acetate=20:1] to give tert-butyl 2-((1-(tert-butoxycarbonyl)-1H-indol-5-yl)amino)-4-phenylbenzoate.

1. temperaturewas heated
2. temperaturerefluxed for 8 hours
3. filtrationinsoluble matter was filtrated
4. additionethyl acetate and 10% citric acid aqueous solution were added to it
5. customThe organic layer was separated
6. washafter washing with saturated sodium chloride aqueous solution
7. customthe solvent was removed under reduced pressure