反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To a mixture of 20 mg of (5,6-dihydro benzo[b]pyrido-[3,2-f]oxepin-8-yl)-acetic acid and 0.5 ml of ethanol was added 2.5 ml of a saturated hydrogen chloride gas-ethanol solution, and the resulting mixture was stirred at room temperature for 1.5 hours. After the completion of the reaction, this was basified with a saturated sodium hydrogen carbonate solution and extracted with chloroform. The extract was washed with a saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was distilled off to obtain an oil, which was chromatographed over 1 g of silica gel and eluted with benzene/chloroform (9/1-8/1), thereby yielding 18 mg (yield: 81.8%) of ethyl(5,6-dihydro benzo[b]pyrido[3,2-f]-oxepin-8-yl)-acetate as a colorless oil.
WORKUP
后处理
- customAfter the completion of the reaction
- extractionextracted with chloroform
- washThe extract was washed with a saturated sodium chloride solution
- dry with materialdried over anhydrous sodium sulfate
- distillationThe solvent was distilled off
- customto obtain an oil, which
- customwas chromatographed over 1 g of silica gel
- washeluted with benzene/chloroform (9/1-8/1)