HRID424620
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 cyclopentanone-3-carboxylic acid (5.00 g, 39 mmol), caesium carbonate (12.82 g, 39 mmol) and ethyl iodide (9.12 g, 4.75 ml, 58.5 mmol) in DMF (50 ml) was stirred at RT for 18 h. The mixture was then concentrated i. vac., the residue was taken up in toluene, the mixture was concentrated again and 2 N hydrochloric acid and EtOAc were then added. The aq. phase was extracted with EtOAc (3×30 ml) and the combined organic phases were washed with aq. sodium thiosulfate soln. The organic phase was dried with Na2SO4 and concentrated i. vac.
WORKUP
后处理
- concentrationThe mixture was then concentrated i
- concentrationthe mixture was concentrated again
- addition2 N hydrochloric acid and EtOAc were then added
- extractionThe aq. phase was extracted with EtOAc (3×30 ml)
- washthe combined organic phases were washed with aq. sodium thiosulfate soln
- dry with materialThe organic phase was dried with Na2SO4
- concentrationconcentrated i