反应详情

温度

80 °C

To a 250 mL round bottomed flask was added 5-bromo-3-chloro-2-methoxypyridine (1.5 g), tribasic potassium phosphate (2.86 g, 13.5 mmol), bis(diphenylphosphino)ferrocene]palladium (II) dichloromethane adduct (0.275 g, 6.74 mmol), tert-butyl 3-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate (Step B, 2.27 g, 7.13 mmol), dioxane (50 mL) and water (3 mL). The flask was sealed and was stirred at 80° C. overnight. The reaction was cooled to room temperature, diluted with ethyl acetate, washed with water, filtered and the filtrate concentrated. The resultant residue was purified by silica gel chromatography to yield tert-butyl 4-(5-chloro-6-methoxypyridin-3-yl)-3-methylbenzoate (2.0 g, 5.99 mmol). LCMS (M+H)+: 334.0

1. customThe flask was sealed
2. temperatureThe reaction was cooled to room temperature
3. washwashed with water
4. filtrationfiltered
5. concentrationthe filtrate concentrated
6. customThe resultant residue was purified by silica gel chromatography