HRID1066350
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 sodium (1.3 g, 52 mmol) in ethanol (50 mL) was added diethyl malonate (8.8 g 55 mmol) followed by 6,9-dichloro-2-methoxyacridine (9.68 g, 35 mmol) and toluene (5 mL). The mixture was heated to reflux for 24 h, diluted with aqueous potassium carbonate, extracted with ethyl acetate, dried, and concentrated in vacuo to give solid which was purified by flash column chromatography (silica gel, 5-12% methanol:dichloromethane) to give the title compound. MS(ES) m/e 402.2 (M+H)+.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureto reflux for 24 h
- extractionextracted with ethyl acetate
- customdried
- concentrationconcentrated in vacuo
- customto give solid which
- customwas purified by flash column chromatography (silica gel, 5-12% methanol:dichloromethane)