HRID1066350

反应详情

EQUATION

反应方程式

HRID 1066350 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 24 h
  3. extractionextracted with ethyl acetate
  4. customdried
  5. concentrationconcentrated in vacuo
  6. customto give solid which
  7. customwas purified by flash column chromatography (silica gel, 5-12% methanol:dichloromethane)