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 solution of 588 mg (0.995 mmol) of the amide compound in methanol (10 ml) was added 190 mg (0.999 mmol) of p-toluenesulfonic acid monohydrate, and the mixture was refluxed for 1 hour. The reaction mixture was diluted with water and adjusted to a pH value of 10 by the addition of aqueous solution of sodium carbonate and then extracted with ethyl acetate. The organic layer was washed with water and concentrated by evaporation under reduced pressure, The residue was subjected to Sephadex column chromatography, eluted with methanol, to give 375 mg (0.746 mmol) of N-[3-(3,5-dimethoxy-4-hydroxyphenyl) -2-propenoyl]-N'-(2-benzhydroxyethyl) piperazine. Spectrophotometric data of the product support the structure shown below. ##STR92##
WORKUP
后处理
- temperaturethe mixture was refluxed for 1 hour
- extractionextracted with ethyl acetate
- washThe organic layer was washed with water
- concentrationconcentrated by evaporation under reduced pressure
- washeluted with methanol