反应详情

温度

115 °C

step 1—A mixture of 3-(3-bromo-5-tert-butyl-phenyl)-2-methoxy-pyridine (123 mg, 0.384 mmol), phenol (46 mg, 0.489 mmol), Pd(OAc)2 (4.1 mg, 0.018 mmol), 2-di-tert-butylphosphino-2′,4′,6′-tri-isopropyl-1,1′-biphenyl (9.9 mg, 0.023 mmol) and K3PO4 (167 mg, 0.787 mmol)) in a Schlenk flask was purged with argon before toluene (5 mL) was added. The reaction under an argon atmosphere was heated overnight at 115° C. The reaction was cooled to RT, filtered through CELITE, and the filtrate was concentrated. The crude residue was purified by SiO2 chromatography eluting with an EtOAc/hexane gradient (0 to 2% EtOAc) to afford 40 mg (41%) of 3-(3-tert-butyl-5-phenoxy-phenyl)-2-methoxy-pyridine (124).

1. customwas purged with argon before toluene (5 mL)
2. additionwas added
3. customThe reaction under an argon atmosphere
4. temperatureThe reaction was cooled to RT
5. filtrationfiltered through CELITE
6. concentrationthe filtrate was concentrated
7. customThe crude residue was purified by SiO2 chromatography
8. washeluting with an EtOAc/hexane gradient (0 to 2% EtOAc)