反应详情

A mixture of 4-methylphenylboronic acid (0.65 g, 4.3 mmol), t-butyl-3-iodobenzoate (0.87 g, 2.86 mmol), K2CO3 (0.59 g, 4.3 mmol), and (Ph3P)4 Pd (0.17 g, 0.14 mmol) in DME (15 mL) was degassed and flushed with N2 before being brought to reflux for 2 h. Following a standard aqueous/EtOAc work-up, the residue was triturated with 1:10 EtOAc/hexane. The excess boronic acid was removed by filtration, and the filtrate was concentrated to give an oil which was purified by flash chromatography (hexane) to give an oil (0.6 g). This material (≈60% pure) was used as such for the next step.

1. customwas degassed
2. customflushed with N2
3. temperatureto reflux for 2 h
4. customthe residue was triturated with 1:10 EtOAc/hexane
5. customThe excess boronic acid was removed by filtration
6. concentrationthe filtrate was concentrated
7. customto give an oil which
8. customwas purified by flash chromatography (hexane)