反应详情

温度

90 °C

Under an argon atmosphere, to 4 ml 1,2-dimethoxyethane are added 5-bromo-pyridine-2-carboxylic acid (93 mg, 0.46 mmol), 4-(2-carboxyethyl)benzeneboronic acid (106 mg, 0.55 mmol), 0.51 ml of a 2M aqueous sodium carbonate solution and dichlorobis-(triphenylphosphin) palladium (II) (20 mg, 0.03 mmol). The mixture is stirred at 90° C. overnight, cooled and quenched with water. Ethyl acetate is added and the mixture adjusted to pH=2 with 1M hydrochloric acid. After threefold extraction with ethyl acetate, the combined organic layers are dried over magnesium sulfate, filtered, and evaporated in vacuo. The residue is purified by silica gel chromatography (eluent:dichloromethane/methanol 5:1).

1. temperaturecooled
2. customquenched with water
3. additionEthyl acetate is added
4. extractionAfter threefold extraction with ethyl acetate
5. dry with materialthe combined organic layers are dried over magnesium sulfate
6. filtrationfiltered
7. customevaporated in vacuo
8. customThe residue is purified by silica gel chromatography (eluent:dichloromethane/methanol 5:1)