HRID238161
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
- 90 °C
PROCEDURE
实验过程
Under argon, 4.2 g (15.15 mmol) of tert-butyl 1-(4-bromobutyl)cyclopropanecarboxylate were initially charged in 50 ml of DMF, 3.34 g (22.72 mmol) of phthalimide and 4.19 g (30.3 mmol) of potassium carbonate were added and the mixture was stirred at 90° C. for 2 h. The reaction mixture was then filtered, and the filtrate was diluted with water and extracted three times with ethyl acetate. The combined organic phases were dried over magnesium sulfate and concentrated under reduced pressure. The product was purified by chromatography on silica gel (mobile phase cyclohexane/ethyl acetate 10:1). This gave 4.23 g (81.3% of theory) of the target compound.
WORKUP
后处理
- filtrationThe reaction mixture was then filtered
- additionthe filtrate was diluted with water
- extractionextracted three times with ethyl acetate
- dry with materialThe combined organic phases were dried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe product was purified by chromatography on silica gel (mobile phase cyclohexane/ethyl acetate 10:1)