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 230 ml of dimethylformamide were added 25 g of homopiperazine and 5.4 g of sodium bicarbonate and then 25 ml of water followed by dropwise addition of 10 g of benzyloxycarbonyl chloride with stirring under ice cooling, and the mixture was stirred at a room temperature overnight. After evaporating off dimethylformamide under a reduced pressure, the reaction mixture was extracted three times with 100 ml of chloroform, and the extract was dried over magnesium sulfate and evaporated to remove the solvent under a reduced pressure. The resulting residue was applied to a silica gel column and eluted with chloroform/methanol (9:1), to obtain 9 g of the title compound as a light yellow liquor liquid.
WORKUP
后处理
- stirringthe mixture was stirred at a room temperature overnight
- customAfter evaporating off dimethylformamide under a reduced pressure
- extractionthe reaction mixture was extracted three times with 100 ml of chloroform
- dry with materialthe extract was dried over magnesium sulfate
- customevaporated
- customto remove the solvent under a reduced pressure
- washeluted with chloroform/methanol (9:1)