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 10 ml flask, 3,4-dihydro-2H-pyrido[4,3-b][1,4]oxazine (150 mg, 1.102 mmol) and 3-chloro-4-methoxy-benzoyl chloride (249 mg, 1.212 mmol) were dissolved in dichloromethane. Triethylamine (0.77 ml, 5.510 mmol) was added thereto and then stirred at room temperature for 2 hours. The reaction mixture was neutralized with 1N hydrochloric acid solution and extracted with dichloromethane. And the combined organic layer was dried over anhydrous magnesium sulfate (MgSO4), filtered and evaporated under reduced pressure. The residue was purified by column chromatography on silica eluting with a solvent of ethyl acetate. The fractions containing the product were collected and evaporated to obtain ivory-colored solid (238 mg, 71%).
WORKUP
后处理
- extractionextracted with dichloromethane
- dry with materialAnd the combined organic layer was dried over anhydrous magnesium sulfate (MgSO4)
- filtrationfiltered
- customevaporated under reduced pressure
- customThe residue was purified by column chromatography on silica eluting with a solvent of ethyl acetate
- additionThe fractions containing the product
- customwere collected
- customevaporated