HRID649174
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 90 °C
PROCEDURE
实验过程
7.02 Grams of 3-methyl-5,6,7,8-tetrahydroquinoline-N-oxide was dissolved in acetic anhydride, and the solution was heated at 90° C. with stirring for 3.5 hours. Acetic anhydride was removed by evaporation under reduced pressure, then an aqueous solution of sodium carbonate was added to make the residue alkaline and was extracted with chloroform. The chloroform layer was washed with an aqueous solution saturated with sodium chloride, then dried with anhydrous magnesium sulfate. The solvent was removed by evaporation, and the residue thus obtained was purified by a silica gel column chromatography (eluent: dichloromethane) to obtain 7.18 g of 3-methyl-8-acetoxy-5,6,7,8-tetrahydroquinoline.
WORKUP
后处理
- customAcetic anhydride was removed by evaporation under reduced pressure
- additionan aqueous solution of sodium carbonate was added
- extractionwas extracted with chloroform
- washThe chloroform layer was washed with an aqueous solution saturated with sodium chloride
- dry with materialdried with anhydrous magnesium sulfate
- customThe solvent was removed by evaporation
- customthe residue thus obtained
- customwas purified by a silica gel column chromatography (eluent: dichloromethane)