HRID2036088
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
- 80 °C
PROCEDURE
实验过程
5-Benzyl-1-oxa-5-azaspiro[2.4]heptane (946 mg) was dissolved in acetonitrile (30 mL), and aniline (0.55 mL) and lithium perchlorate (640 mg) were added. After stirring at 80° C. overnight, the solvent was evaporated under reduced pressure. The residue was dissolved in ethyl acetate, and the solution was washed twice with aqueous sodium hydrogen carbonate solution. The organic layer was dried over sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography using basic silica gel (20% ethyl acetate/hexane to 60% ethyl acetate/hexane) to give the object product (768 mg, 54%).
WORKUP
后处理
- customthe solvent was evaporated under reduced pressure
- dissolutionThe residue was dissolved in ethyl acetate
- washthe solution was washed twice with aqueous sodium hydrogen carbonate solution
- dry with materialThe organic layer was dried over sodium sulfate
- customthe solvent was evaporated under reduced pressure
- customThe residue was purified by silica gel column chromatography