関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 3-Bromophenol | HCID 11563 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Hexane, 2,5-dichloro-2,5-dimethyl- | HCID 80360 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Bromo-5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalen-1-ol | HCID 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
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06849658B2 |
|---|
| 出典データセット | uspto-grants-2005_02 |
|---|
| ORD ID | ord-99e55126c38b44819539451eb4d235a6 |
|---|
| 出典メモ | uspto-grants-2005_02 |
|---|