HRID616028
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
- 20 °C
PROCEDURE
实验过程
A mixture of 8 g of 3-(3',4'-dimethoxyphenyl)-piperidine, 80 ml of benzene and 3.6 ml of acetic acid anhydride was stirred at 20° C for an hour and was then diluted with 100 ml of water. 500 ml of an aqueous solution saturated with sodium bicarbonate were added thereto and the mixture was stirred for an hour and then was decanted. The aqueous phase was re-extracted with ethyl acetate and the organic phases were washed with water, dried and evaporated to dryness. The residue was chromatographed over silica gel and was eluted with a 6-3-1 cyclohexane-chloroform-triethylamine mixture to obtain 6.75 g of N-acetyl-3-(3',4'-dimethoxyphenyl)-piperidine.
WORKUP
后处理
- stirringthe mixture was stirred for an hour
- customwas decanted
- extractionThe aqueous phase was re-extracted with ethyl acetate
- washthe organic phases were washed with water
- customdried
- customevaporated to dryness
- customThe residue was chromatographed over silica gel
- washwas eluted with a 6-3-1 cyclohexane-chloroform-triethylamine mixture