HRID1257428
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
- 120 °C
PROCEDURE
实验过程
The compound (0.73 g) obtained in Example 124a was dissolved in phosphorus oxychloride (10 mL), and the mixture was stirred at 110-130° C. overnight with heating. The reaction mixture was cooled to room temperature, slowly poured into water, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography (carrier: silica gel, eluent: petroleum ether-ethyl acetate) to give the title compound (0.50 g) as a colorless solid.
WORKUP
后处理
- temperaturewith heating
- temperatureThe reaction mixture was cooled to room temperature
- extractionthe mixture was extracted with ethyl acetate
- dry with materialThe ethyl acetate layer was dried over sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by column chromatography (carrier: silica gel, eluent: petroleum ether-ethyl acetate)