HRID1306

反应详情

EQUATION

反应方程式

HRID 1306 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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).

WORKUP

后处理

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