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 2 ml anhydrous dichloromethane solution of 87.2 mg (0.2 mmol) of the compound obtained in Example 48, 26.6 μl (0.24 mmol) of N-methylpiperazine and 70 μl (0.5 mmol) of triethylamine were added, and the mixture was stirred at room temperature for 20 hours. Then, water was added to the reaction mixture, and the mixture was extracted with dichloromethane. The organic layer was washed with water and a saturated aqueous solution of sodium chloride. After the washed layer was dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (chloroform/methanol=50/1˜30/1) to obtain 87 mg (87%) of the captioned compound.
WORKUP
后处理
- extractionthe mixture was extracted with dichloromethane
- washThe organic layer was washed with water
- dry with materialAfter the washed layer was dried over anhydrous sodium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was purified by silica gel column chromatography (chloroform/methanol=50/1˜30/1)