HRID716450

反应详情

EQUATION

反应方程式

HRID 716450 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 8.61 g (20.0 mmol) of 5-isopropyl-2-methyl-6-(pentafluorophenoxy)-7-phenyl-1H-indene in 200 ml of THF cooled to −25° C., 885 mg (22.1 mmol) of potassium hydride was added. The resulting mixture was stirred overnight at room temperature, filtered through glass frit (G3) to remove an excess of KH, then cooled to −25° C., and 13.0 g (101 mmol, 5 eq.) of dichlorodimethylsilane was added in one portion. The resulting solution was stirred overnight at room temperature, then evaporated to dryness. The residue was dissolved in 200 ml of toluene, and the formed suspension was filtered through glass frit (G3). The precipitate was additionally washed by 2×30 ml of toluene. The combined filtrate was evaporated to dryness to give 10.5 g (99%) of the title product which was further used without an additional purification.

WORKUP

后处理

  1. filtrationfiltered through glass frit (G3)
  2. customto remove an excess of KH
  3. temperaturecooled to −25° C.
  4. stirringThe resulting solution was stirred overnight at room temperature
  5. customevaporated to dryness
  6. dissolutionThe residue was dissolved in 200 ml of toluene
  7. filtrationthe formed suspension was filtered through glass frit (G3)
  8. washThe precipitate was additionally washed by 2×30 ml of toluene
  9. customThe combined filtrate was evaporated to dryness