反应详情

To 1-fluoro-2-iodobenzene 0.11 g were added 2-dicyclohexylphosphino-2′,4′,6′-triisopropylbiphenyl 9.5 mg, tris(dibenzylideneacetone)dipalladium(0) 3.7 mg, palladium acetate 0.90 mg, tert-butyl 2-amino-4-phenethylbenzoate 59 mg, cesium carbonate 0.13 g and toluene 1.0 mL at room temperature, and it was heated and refluxed for 9 hours and 30 minutes. After the reaction mixture was cooled to room temperature, ethyl acetate and 1.0 mol/L hydrochloric acid 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 [Fuji SILYSIA Chemical Ltd., PSQ100B(spherical type), eluent; hexane:ethyl acetate=200:1] to give tert-butyl 2-(2-fluoroanilino)-4-phenethylbenzoate 62 mg of a colorless oil.

1. temperatureit was heated
2. temperaturerefluxed for 9 hours and 30 minutes
3. customThe organic layer was separated
4. customcollected
5. dry with materialdried over anhydrous magnesium sulfate
6. washafter washing with saturated sodium chloride aqueous solution
7. customthe solvent was removed under reduced pressure