HRID2301140
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
5,6,7,8-Tetrahydroquinoline N-oxide (1.6 g, 11 mmol) was mixed with acetic anhydride (9.2 ml) and stirred at 90° C. for 7 hours. After removing the solvent by evaporation under a reduced pressure, the residue was neutralized with sodium hydroxide aqueous solution (1 N) and the reaction product was extracted with chloroform. The extract was washed with saturated brine and dried with anhydrous sodium sulfate, and then the solvent was removed by evaporation under a reduced pressure and the thus obtained material was separated and purified by a silica gel column chromatography to obtain 690 mg (3.6 mmol, 33%) of the title compound.
WORKUP
后处理
- customAfter removing the solvent
- customby evaporation under a reduced pressure
- extractionthe reaction product was extracted with chloroform
- washThe extract was washed with saturated brine
- dry with materialdried with anhydrous sodium sulfate
- customthe solvent was removed by evaporation under a reduced pressure
- customthe thus obtained material was separated
- custompurified by a silica gel column chromatography