HRID2240188
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 solution of 11-(3-fluorophenyl)-9-methoxy-3,4-dihydro-2H-pyrido[1,2-b]isoquinoline-1,6-dione (125 mg) in 4 mL pyridine was added hydroxylamine hydrochloride (51 mg). The reaction was heated to reflux for 5 h, then cooled to room temp and partitioned between ether and water. The aqueous solution was extracted with ether (2×). The combined organic solutions were washed with 1 N HCl (1×), and 10% bicarb (1×), then dried (MgSO4) and concentrated. Flash chromatography (10-70% EtOAc/hexanes) gave the titled compound.
WORKUP
后处理
- temperatureThe reaction was heated
- temperatureto reflux for 5 h
- custompartitioned between ether and water
- extractionThe aqueous solution was extracted with ether (2×)
- washThe combined organic solutions were washed with 1 N HCl (1×), and 10% bicarb (1×)
- dry with materialdried (MgSO4)
- concentrationconcentrated