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HRID 41845作成日:2026年10月24日

Sulfuric Acid → 1-Ethyl-4-trifluoromethylcyclohexanol

https://huagongshe.com/ja/reaction/41845

反応式

関与物質

役割名称HCID仕込み量
反応物Sulfuric AcidHCID 1118—
反応物Ethyl BromideHCID 6332—
反応物4-(Trifluoromethyl)cyclohexanoneHCID 2777491—
反応物MagnesiumHCID 5462224—
溶媒TetrahydrofuranHCID 8028—
生成物1-Ethyl-4-trifluoromethylcyclohexanolHCID 6475651170%

反応条件

温度-5 °C

反応手順

The inside of a reactor was sufficiently dried by vacuum heating, and the atmosphere inside the reactor was replaced with dry nitrogen. The reactor was charged with a Grignard reagent that was prepared in 350 ml of dehydrated tetrahydrofuran (dehydrated THF) using 9.7 g (0.40 mol) of a magnesium powder and 38.9 g (0.36 mol) of bromoethane 50 ml of a dehydrated THF solution of 49.8 g (0.30 mol) of 4-trifluoromethylcyclohexanone was added to the reactor over 15 minutes with stirring while cooling the solution at −5° C. using an ice bath. After increasing the temperature of the reactor to room temperature, the mixture was stirred for 2 hours. 500 ml of ice water and 100 ml of ice-cooled diluted sulfuric acid were then added to the mixture while sufficiently stirring the mixture. After separating the THF layer, the aqueous layer was extracted with diethyl ether to obtain an extract. The extract was combined with the THF layer, sequentially washed with a 5% sodium carbonate aqueous solution and water, and dried over sodium sulfate (desiccating agent). After removing sodium sulfate using a Buchner funnel, the organic solvent was evaporated. The residue was distilled under reduced pressure (30 mmHg). 1-Ethyl-4-trifluoromethylcyclohexanol was thus obtained (41.2 g (yield: 70%)).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08535871B2
出典データセットuspto-grants-2013_09
ORD IDord-3eda108bfce74d3d871703601a0114d2
出典メモuspto-grants-2013_09