反应详情

温度

80 °C

To a suspension of 1 g (1.96 mmol) of methyl 6-[3-[(4-methoxybenzyl)oxy]-4-chlorophenyl]-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine-2-carboxylate and 0.58 g (2.55 mmol) of 2-bromo-3,5-dichloropyridine in 10 mL of a 2/1 DME/water mixture, argon is sparged through for 10 minutes, followed by successive addition of 0.81 g (5.88 mmol) of K2CO3 and 0.159 g (0.14 mmol) of Pd(PPh3)4. The reaction mixture is heated for 4 hours at 80° C. and then cooled and diluted in 50 mL of EtOAc. The organic phase is washed with 2×20 mL of water, dried over Na2SO4 and then concentrated under reduced pressure. The residue is then purified on a column of silica gel, eluting with a cyclohexane/EtOAc gradient of from 0 to 40% EtOAc, to give 0.4 g of methyl 2′-[3-[(4-methoxybenzyl)oxy]-4-chlorophenyl]-3,5-dichloro-2,3′-bipyridine-6′-carboxylate in the form of an oil.

1. customis sparged through for 10 minutes
2. temperaturecooled
3. washThe organic phase is washed with 2×20 mL of water
4. dry with materialdried over Na2SO4
5. concentrationconcentrated under reduced pressure
6. customThe residue is then purified on a column of silica gel
7. washeluting with a cyclohexane/EtOAc gradient of from 0 to 40% EtOAc