HRID650305

反应详情

EQUATION

反应方程式

HRID 650305 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-20 °C

PROCEDURE

实验过程

20 ml of triethylamine, 2.88 g (20 mmole) of 4,7-dimethyl-indene, 4.08 g (20 mmole) of iodobenzene and 0.134 g (0.6 mmole) of Pd(OAc)2 were stirred under reflux for 12 h. After it all the triethylamine was removed under reduced pressure. The residue was treated with the mixture 50 ml of water and 50 ml of diethyl ether. Etherial layer was separated, washed twice with water, filtered and dried over Na2SO4. Ether was removed and some 20 ml of pentane were added to the reaction mixture. It was cooled down to −20° C. and product was crystallized as white crystals, which were filtered, washed with small portion of cold pentane and dried in vacuum. The yield of product was 38%.

WORKUP

后处理

  1. temperatureunder reflux for 12 h
  2. customAfter it all the triethylamine was removed under reduced pressure
  3. additionThe residue was treated with the mixture 50 ml of water and 50 ml of diethyl ether
  4. customEtherial layer was separated
  5. washwashed twice with water
  6. filtrationfiltered
  7. dry with materialdried over Na2SO4
  8. customEther was removed
  9. additionsome 20 ml of pentane were added to the reaction mixture
  10. customproduct was crystallized as white crystals, which
  11. filtrationwere filtered
  12. washwashed with small portion of cold pentane
  13. customdried in vacuum