HRID1739645

反应详情

EQUATION

反应方程式

HRID 1739645 的结构方程式

CONDITIONS

反应条件

温度
-20 °C

PROCEDURE

实验过程

4.45 g (20 mmol) of 2,2-(cyclopentadienyl)(indenyl)propane was dissolved in 100 ml of ether, cooled up to -20° C., and treated by 22 ml of 2.0M n-BuLi/pentane. The resulting suspension was allowed to warm to room temperature, then cooled to -40° C., and treated with 12.06 g (50 mmol) of Et2SnCl. Organic layer was separated, evaporated, and mixed with 50 ml of toluene. 4.66 g (20 mmol) of ZrCl4 was added, and the mixture was stirred for 6 hours under 80° C. Toluene was removed, the crude product was recrystallized from THF. 5.97 g of the product was obtained (yield 78%).

WORKUP

后处理

  1. temperatureto warm to room temperature
  2. temperaturecooled to -40° C.
  3. additiontreated with 12.06 g (50 mmol) of Et2SnCl
  4. customOrganic layer was separated
  5. customevaporated
  6. additionmixed with 50 ml of toluene
  7. customToluene was removed
  8. customthe crude product was recrystallized from THF