HRID2080729
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
The compound (123 mg) obtained in Example 7-4 was dissolved in xylene (5.0 ml). A xylene solution (5.0 ml) containing the compound (83.4 mg) obtained in Example 1-2 was dropped to the solution and the whole was refluxed under heating for 63 hours. The solution was added with water to stop the reaction and then subjected to extraction with chloroform. The organic layer was washed with water and a saturated saline solution, followed by drying with anhydrous sodium sulfate. The residue obtained by distilling the solvent off was then purified through silica gel column chromatography (hexane/ethyl acetate), thereby obtaining the subject compound (88.4 mg) as a yellow solid.
WORKUP
后处理
- additionwas dropped to the solution
- temperaturethe whole was refluxed
- temperatureunder heating for 63 hours
- customthe reaction
- extractionsubjected to extraction with chloroform
- washThe organic layer was washed with water
- dry with materialby drying with anhydrous sodium sulfate
- customThe residue obtained
- distillationby distilling the solvent
- customoff was then purified through silica gel column chromatography (hexane/ethyl acetate)