反应详情

To toluene 4.0 mL solution of tert-butyl 4-bromo-2-(4-fluoroanilino)benzoate 0.20 g were added ethanol 1.2 mL, water 0.60 mL, 4-(hydroxymethyl)phenylboronic acid 91 mg, sodium hydrogen carbonate 0.12 g and tetrakis(triphenylphosphine)palladium(0) 35 mg at room temperature, and it was heated and refluxed under nitrogen atmosphere for 6 hours. After the reaction mixture was cooled to room temperature, water was 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=2:1] to give tert-butyl 2-(4-fluoroanilino)-4-(4-(hydroxymethyl)phenyl)benzoate 64 mg of a pale yellow solid.

1. temperatureit was heated
2. temperaturerefluxed under nitrogen atmosphere for 6 hours
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