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 10.0 g (20.1 mmol) of said 1-benzhydryl-4-(5-(2,3,4-trimethoxyphenyl)-2,4-pentadienoyl)piperazine was added 250 ml of dry ether, and the mixture was stirred. After addition of 760 mg (20.1 mmol) of lithium aluminum hydride, the mixture was heated under reflux for 1 hour To the reaction mixture were added a saturated aqueous solution of ammonium chloride followed by extraction with ether. The organic layer was washed with a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate and concentrated under reduced pressure There was obtained a residue, which was subjected to column chromatography on silica gel to give 9.40 g (19.4 mmol) of 1-benzhydryl-4-(5-(2,3,4-trimethoxyphenyl)-2,4-pentadienyl)piperazine. Spectrophotometric data of the product support the structure (VIII). ##STR8##
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureunder reflux for 1 hour To the reaction mixture
- extractionfollowed by extraction with ether
- washThe organic layer was washed with a saturated aqueous sodium chloride solution
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThere was obtained a residue, which