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HRID 1029067作成日:2026年10月27日

Methyl iodide → 2-iodo-9,9-dimethyl-9H-fluorene

https://huagongshe.com/reaction/1029067

反応式

関与物質

役割名称HCID仕込み量
反応物Methyl iodideHCID 6328—
反応物2-Iodo-9H-fluoreneHCID 224094—
反応物Potassium tert-butoxideHCID 23665647—
溶媒Dimethyl SulfoxideHCID 679—
溶媒TetrahydrofuranHCID 8028—
生成物2-iodo-9,9-dimethyl-9H-fluoreneHCID 11023630—

反応条件

温度25 °C

反応手順

20 parts of 2-iodofluorene was dissolved in a mixed solution of 114 parts of dimethyl sulfoxide (DMSO) and 23 parts of tetrahydrofuran (THF), and the thus obtained mixture was then stirred at 25° C. for 10 minutes. Thereafter, while stirring, 8.7 parts of potassium-tert-butoxide was added to the mixture. Twenty minutes later, 13.2 parts of methyl iodide was added to the mixture, and further twenty minutes later, 8.7 parts of potassium-tert-butoxide was added thereto. Further, twenty minutes later, 13.2 parts of methyl iodide was added thereto, and the obtained mixture was then stirred at 25° C. for 2 hours. After completion of the stirring, the THF was distilled away from the reaction solution, and it was then extracted with toluene-water. The toluene phase was dried over magnesium sulfate, and the toluene was then distilled away, thereby obtaining a brown tarry solid. This brown tarry solid was separated and purified by column chromatography (hexane-ethyl acetate) to obtain 21 parts of 9,9-dimethyl-2-iodofluorene in the form of a colorless crystal.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08735720B2
出典データセットuspto-grants-2014_05
ORD IDord-f80058a1a4d944119bb48b99cee66038
出典メモuspto-grants-2014_05