HRID1766670

反应详情

EQUATION

反应方程式

HRID 1766670 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

4-(4-benzyloxy-3-iodo-phenoxy)-5-methyl-7-nitroindane (571 mg), 3-vinylcyclopentanone (197 μL), palladium acetate (II)(13 mg), triphenylphosphine (30 mg), and silver carbonate (189 mg) were stirred at 80° C. for 21 hours. To the reaction mixture were added water and ethyl acetate. The insoluble material was removed by filtration. The filtrate was extracted with ethyl acetate. The organic layer was washed with 1 mol/L hydrochloric acid, brine successively, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: hexane/ethyl acetate=10/1−5/1) to give the title compound (155 mg).

WORKUP

后处理

  1. customThe insoluble material was removed by filtration
  2. extractionThe filtrate was extracted with ethyl acetate
  3. washThe organic layer was washed with 1 mol/L hydrochloric acid, brine successively
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customThe residue was purified by column chromatography on silica gel (eluent: hexane/ethyl acetate=10/1−5/1)