HRID424620

反应详情

EQUATION

反应方程式

HRID 424620 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationThe mixture was then concentrated i
  2. concentrationthe mixture was concentrated again
  3. addition2 N hydrochloric acid and EtOAc were then added
  4. extractionThe aq. phase was extracted with EtOAc (3×30 ml)
  5. washthe combined organic phases were washed with aq. sodium thiosulfate soln
  6. dry with materialThe organic phase was dried with Na2SO4
  7. concentrationconcentrated i