HRID592301
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 110 °C
PROCEDURE
实验过程
To a solution of tert-butyl 8-chloro-3-pyridin-2-yl[1,2,4]triazolo[4,3-a]pyridine-6-carboxylate (0.5 g, 1.51 mmol) in toluene (12 mL) were added (4-fluorophenyl)boronic acid (0.32 g, 2.27 mmol), 2-dicyclohexylphosphino-2′,4′,6′-triisopropylbiphenyl (72.1 mg, 0.15 mmol), palladium(II) acetate (33.9 mg, 0.15 mmol) and potassium phosphate tribasic (0.96 g, 4.53 mmol). The mixture was heated to 110° C. After 2 h, the mixture was cooled to ambient temperature, filtered with Celite and the filtrate was concentrated. Purification by silica gel chromatography (100% dichloromethane→60% dichloromethane/ethyl acetate) gave of the title compound (0.53 g): LC-MS [M+1]=391.2.
WORKUP
后处理
- temperaturethe mixture was cooled to ambient temperature
- filtrationfiltered with Celite
- concentrationthe filtrate was concentrated
- customPurification by silica gel chromatography (100% dichloromethane→60% dichloromethane/ethyl acetate)