HRID704416
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
A solution of 1-bromo-3-methyl-3-phenylbutane (0.73 g), ethyl piperazinecarboxylate (0.51 g) and anhydrous potassium carbonate (0.50 g) in tetrahydrofuran (5 ml) was refluxed under heating for 36 hours. To the reaction solution was added water and the solution was extracted with ethyl acetate. After washing with a saturated aqueous solution of sodium chloride, the ethyl acetate layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resultant residue was subjected to silica gel column chromatography (15 g) and elution with a hexane-ethyl acetate (2:1) mixture gave 0.80 g of ethyl 4-(3-methyl-3-phenylbutyl)piperazine-1-carboxylate.
WORKUP
后处理
- temperatureunder heating for 36 hours
- extractionthe solution was extracted with ethyl acetate
- washAfter washing with a saturated aqueous solution of sodium chloride
- dry with materialthe ethyl acetate layer was dried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
- washThe resultant residue was subjected to silica gel column chromatography (15 g) and elution with a hexane-ethyl acetate (2:1) mixture