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HRID 271025作成日:2026年10月25日

Hexane → 1-(3-(1,1-Dimethylpropyl)cyclopentadienyl)-1-(3,6-di-tert-butylfluorenyl)cyclohexane

https://huagongshe.com/reaction/271025

反応式

関与物質

役割名称HCID仕込み量
反応物HexaneHCID 8058—
反応物3,6-DI-Tert-butylfluoreneHCID 11140437—
反応物3-(1,1-Dimethylpropyl)-6,6-dimethylfulveneHCID 17818147—
反応物ButyllithiumHCID 178418339—
溶媒WaterHCID 962—
溶媒Diethyl EtherHCID 3283—
溶媒TetrahydrofuranHCID 8028—
生成物1-(3-(1,1-Dimethylpropyl)cyclopentadienyl)-1-(3,6-di-tert-butylfluorenyl)cyclohexaneHCID 13172514145%

反応手順

To a solution of 2.38 g (8.5 mmol) of 3,6-di-tert-butylfluorene in 40 ml of THF, 5.7 ml (9.2 mmol) of a hexane solution of n-butyllithium was dropwise added in a nitrogen atmosphere with ice cooling, followed by stirring at room temperature for one night. To the resulting red solution, a solution of 2.00 g (9.2 mmol) of 3-(1,1-dimethylpropyl)-6,6-dimethylfulvene in 30 ml of THF was dropwise added in a nitrogen atmosphere with ice cooling, followed by stirring at room temperature for one night. After the reaction solution was diluted with 100 ml of ether, 50 ml of water was added. The separated organic phase was washed with water and a saturated saline solution, then dried over magnesium sulfate and filtered. From the filtrate, the solvent was removed under reduced pressure to obtain a liquid. The liquid was isolated and purified by column chromatography (silica gel, developing solvent: hexane) to obtain 1.88 g (3.80 mmol) of a white solid (yield: 45%). The analyzed values are given below.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07449533B2
出典データセットuspto-grants-2008_11
ORD IDord-5375b988de2d4f0699d927681af91b4e
出典メモuspto-grants-2008_11