HRID2240185
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
PROCEDURE
实验过程
To a mixture of 2-(3-fluorobenzoyl)-4-methoxybenzoyl chloride (3.36 g) and piperidin-3-one hydrochloride (1.88 g) in 54 ml of toluene was added 2,6-lutidine (4.01 ml). The reaction was heated at reflux (3:10 pm) for 24 h, then partitioned between EtOAc and 400 mL of 1 N HCl. The aqueous solution was extracted twice more with EtOAc. The combined organic solutions were dried (MgSO4) and concentrated. Flash chromatography (40-100% EtOAc/hexanes) to gave the titled compound.
WORKUP
后处理
- temperatureThe reaction was heated
- temperatureat reflux (3:10 pm) for 24 h
- custompartitioned between EtOAc and 400 mL of 1 N HCl
- extractionThe aqueous solution was extracted twice more with EtOAc
- dry with materialThe combined organic solutions were dried (MgSO4)
- concentrationconcentrated