反应详情

Methyl 3-bromobenzoate (1.99 g, 9.25 mmol), tetrakis(triphenylphosphine) palladium(O) (110 mg), sodium carbonate (2.04 g, 19 mmol in 5 ml water) and toluene (10 ml) were degassed under nitrogen in a 25 ml flask fitted with a reflux condenser. 2-Methoxybenzeneboronic acid (1.46 g, 9.61 mmol) in toluene (1 ml) was added and the mixture was heated at reflux for two days then mixed with 1:1 saturated sodium chloride/ethyl acetate (15 ml). The organic materials were separated, dried (MgSO4) then concentrated under reduced pressure. The residue was purified by flash chromatography (SiO2, gradient hexane to 8:1 hexane/ethyl acetate) which gave methyl 3-(2-methoxyphenyl)benzoate (1.43 g, 64%), m.p.: 92°-93° C.

1. customfitted with a reflux condenser
2. temperaturethe mixture was heated
3. temperatureat reflux for two days
4. customThe organic materials were separated
5. dry with materialdried (MgSO4)
6. concentrationthen concentrated under reduced pressure
7. customThe residue was purified by flash chromatography (SiO2, gradient hexane to 8:1 hexane/ethyl acetate) which