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
- 100 °C
PROCEDURE
实验过程
The 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (273 mg, 0.472 mmol), 2,4-dichloro-5,7-difluoro-3-methylquinoline (XantPhos) (780 mg, 3.20 mmol), 5,5-dimethylpiperidin-2-one (400 mg, 3.20 mmol), cesium carbonate (1.40 g, 4.40 mmol) and Pd2(dba)3 (140 mg, 0.160 mmol) were slurried in 1,4-dioxane (8.5 mL) and heated in a microwave reactor at 100° C. for 3 h. The reaction was cooled and then diluted with EtOAc and DCM. The slurry was then filtered and the filtrate cond. The residue was purified by medium pressure chromatography (silica gel, 0 to 50% EtOAc:DCM) to give 1-(4-chloro-5,7-difluoro-3-methylquinolin-2-yl)-5,5-dimethylpiperidin-2-one. Mass Spectrum (ESI) m/e=339.1 (M+1).
WORKUP
后处理
- temperatureThe reaction was cooled
- filtrationThe slurry was then filtered
- customThe residue was purified by medium pressure chromatography (silica gel, 0 to 50% EtOAc:DCM)