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HRID 2070697作成日:2026年10月26日

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

https://huagongshe.com/reaction/2070697

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 were introduced into 175 mL of toluene and 13 mL of THF, and 24.6 mL of n-butyllithium (2.5 Min toluene) were added without interruption at room temperature. After this addition was complete, the mixture was heated to 80° C. and stirred at this temperature for one hour. It was allowed to cool to 40° C., then 3.96 g (30.7 mmoles) of dimethyldichlorosilane were slowly added dropwise. After this addition, the reaction solution was stirred for three hours at 60° C. and then overnight at room temperature. 70 mL of water were added and the phases that form were separated. The organic phase was washed with 100 mL of water, and the aqueous phase was extracted three times with a total of 100 mL of toluene. The combined organic phases were dried over magnesium sulfate. After separation of the magnesium sulfate, the solvent was removed and the residue was purified by column chromatography. The desired product was 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US08299287B2
出典データセットuspto-grants-2012_10
ORD IDord-e578723e9e7f4039a4b6fadaa31fb67f
出典メモuspto-grants-2012_10