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
CONDITIONS
反应条件
- 温度
- 250 °C
PROCEDURE
实验过程
4-Oxo-6-methoxy-2,3-dihydrofuro[3,2-c]quinoline (217 mg, 1.0 mmol) was dissolved in 10 ml of diethylene glycol in a pressure tube and of 2-methylaniline (282 μl, 2.5 mmol) was added under nitrogen. The reaction mixture was heated at 250° C. for 15 hours. The reaction mixture was diluted with 20 ml of salt water and the aqueous layer was extracted with methylene chloride (15 ml×3). After layer with water (15 ml×3), the organic layer was dried with anhydrous magnesium sulfate and filtrated to be concentrated under reduced pressure. The residue was purified with ethyl acetate as a development solution according to silica gel chromatography to obtain 260 mg of desired compound as solid in 81% of yield.
WORKUP
后处理
- additionwas added under nitrogen
- extractionthe aqueous layer was extracted with methylene chloride (15 ml×3)
- dry with materialAfter layer with water (15 ml×3), the organic layer was dried with anhydrous magnesium sulfate
- filtrationfiltrated
- concentrationto be concentrated under reduced pressure
- customThe residue was purified with ethyl acetate as a development solution