HRID919789
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
7-(2,4-dimethoxy-benzyl)-4-hydroxy-8-oxo-7,8-dihydro-[2,7]naphthyridine-3-carboxylic acid methyl ester (60 mg, 0.162 mmol) in TFA (3 mL) was refluxed for 16 h. Solvent was evaporated in vacuo, and the residue was partitioned between CH2Cl2 and saturated NaHCO3. The aqueous layer was extracted with 10% MeOH/CH2Cl2 until the layers were free of solid. The organic layers were combined, dried over MgSO4, and concentrated in vacuo. The crude product was purified by silica gel chromatography (0-10% MeOH/CH2Cl2) to give 22 mg of the title compound as a pale brown solid. MS: (+) m/z 221.25 (M+1).
WORKUP
后处理
- customSolvent was evaporated in vacuo
- customthe residue was partitioned between CH2Cl2 and saturated NaHCO3
- extractionThe aqueous layer was extracted with 10% MeOH/CH2Cl2 until the layers
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customThe crude product was purified by silica gel chromatography (0-10% MeOH/CH2Cl2)