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HRID 22993作成日:2026年10月23日

Dichloromethane → 3-Bromo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-1-ol

https://huagongshe.com/ja/reaction/22993

反応式

関与物質

役割名称HCID仕込み量
反応物DichloromethaneHCID 6344—
反応物3-BromophenolHCID 11563—
反応物Ammonium ChlorideHCID 25517—
反応物Hexane, 2,5-dichloro-2,5-dimethyl-HCID 80360—
溶媒WaterHCID 962—
生成物3-Bromo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-1-olHCID 22345465—

反応手順

13.40 g (100.0 mmol) of ammonium chloride and 100 ml of dichloromethane are introduced into a three-necked flask under an argon atmosphere. A solution composed of 34.60 g (199.0 mmol) of 3-bromophenol, 89.00 g (486.0 mmol) of 2,5-dichloro-2,5-dimethylhexane and 300 ml of dichloromethane is added dropwise. The reaction mixture is stirred for sixteen hours at room temperature. The reaction mixture is poured into water and extracted with dichloromethane, the extract is washed with water and the organic phase is separated by settling, dried over magnesium sulphate and evaporated. The residue obtained is purified by chromatography on a silica column eluted with a mixture composed of 80% heptane and 20% dichloromethane. After evaporating the solvents, 30.00 g (53%) of the expected compound are collected in the form of white crystals with a melting point of 93° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06849658B2
出典データセットuspto-grants-2005_02
ORD IDord-99e55126c38b44819539451eb4d235a6
出典メモuspto-grants-2005_02