反应详情

温度

110 °C

A mixture of methyl 3-bromo-4-tert-butylbenzoate (120 mg, 443 μmol), compound C.3 (226 mg, 664 μmol), potassium phosphate (282 mg, 1328 μmol), 2-(dicyclohexylphosphino)-2′,6′-dimethoxy-1,1′-biphenyl (36 mg, 89 μmol) (Aldrich, CAS# 657408-07-6), and tris(dibenzylideneacetone)dipalladium(0) (20 mg, 22 μmol) in toluene (1.0 mL) was stirred overnight at 110° C. The mixture was cooled to room temperature, filtered through a pad of celite with EtOAc rinsings, and concentrated. The crude product was purified by silica gel flash chromatography (0-10% EtOAc/hexane) to afford compound C.4 (63 mg, 39% yield) as a colorless oil. MS ESI (pos.) m/e: 388 (M+H2O), 393 (M+Na).

1. temperatureThe mixture was cooled to room temperature
2. filtrationfiltered through a pad of celite with EtOAc rinsings
3. concentrationconcentrated
4. customThe crude product was purified by silica gel flash chromatography (0-10% EtOAc/hexane)
5. customto afford compound C.4 (63 mg, 39% yield) as a colorless oil