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HRID 1375928作成日:2026年10月27日

Toluene → Dimethyl-bis(2-methyl-1H-inden-1-yl)silane

https://huagongshe.com/reaction/1375928

反応式

関与物質

役割名称HCID仕込み量
反応物TolueneHCID 1140—
反応物DichlorodimethylsilaneHCID 6398—
反応物1H-Indene, 2-methyl-HCID 16587—
反応物ButyllithiumHCID 178418339—
溶媒WaterHCID 962—
溶媒TetrahydrofuranHCID 8028—
生成物Dimethyl-bis(2-methyl-1H-inden-1-yl)silaneHCID 4050248—

反応条件

温度80 °C

反応手順

8.0 g (61.4 mmoles) of 2-methylindene are introduced into 175 mL of toluene and 13 mL of THF, and 24.6 mL of n-butyllithium (2.5 M in toluene) are added without interruption at room temperature. After this addition is complete, the mixture is heated to 80° C. and stirred at this temperature for one hour. It is allowed to cool to 40° C., then 3.96 g (30.7 mmoles) of dimethyldichlorosilane are slowly added dropwise. After this addition, the reaction solution is stirred for three hours at 60° C. and then overnight at room temperature. 70 mL of water are added and the phases that form are separated. The organic phase is washed with 100 mL of water, and the aqueous phase is extracted three times with a total of 100 mL of toluene. The combined organic phases are dried over magnesium sulfate. After separation of the magnesium sulfate, the solvent is removed and the residue is purified by column chromatography. The desired product is isolated in a yield of 8.16 g (84%) (purity 99%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07169864B2
出典データセットuspto-grants-2007_01
ORD IDord-d3b03266a7394bfaa66e3536a76eb3fd
出典メモuspto-grants-2007_01