反応 #1402

ord-68a3f07b1c044ef79787604ed33c105d

反応方程式

Cc1cc(C)c([Si](Cl)(Cl)c2c(C)cc(C)cc2C)c(C)c1
dimesityldichlorosilane
C1=Cc2ccccc2C1
indene
[Li][CH2]CCC
butyllithium
Cc1cc(C)c([Si](c2c(C)cc(C)cc2C)(C2C=Cc3ccccc32)C2C=Cc3ccccc32)c(C)c1
dimesitylbis(indenyl)silane

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the mixture was refluxed for 4 hours
  2. 2
    抽出Decomposition of the batch with water, extraction with diethyl ether and chromatography on SiO2 using 2:1 toluene/hexane

実験手順

7 g of indene in 50 cm3of THF were reacted with 24 cm3 of butyllithium (2.5-molar in hexane) at 0° C. under inert conditions. The mixture was heated to room temperature, added dropwise to a solution of 10 g of dimesityldichlorosilane in 40 cm3 of THF, and the mixture was refluxed for 4 hours. Decomposition of the batch with water, extraction with diethyl ether and chromatography on SiO2 using 2:1 toluene/hexane gave 3.28 g of dimesitylbis(indenyl)silane as a solid. MS(m/e,I rel %): 496 (100, M+); 1H NMR in CDCl3 : 2.22 ppm (12 H, s), 2.27 ppm (6 H, s), 3.40 ppm (4 H, s), 6.8-7.4 ppm (14 H, m).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05723705uspto-grants-1998_03