関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 1,1-Dimethylcyclohexane | HCID 11549 | — |
| 反応物 | 1-Bromo-4-(1,1-dimethoxyethyl)benzene | HCID 10911782 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Cyclohexane | HCID 8078 | — |
| 生成物 | 1-[4-(1,1-Dimethoxyethyl)phenyl]-4,4-dimethylcyclohexanol | HCID 18402528 | — |
反応手順
328 ml of a 1.6 M solution of butyllithium in cyclohexane are added at −78° C. to 117 g of 1-bromo-4-(1,1-dimethoxyethyl)benzene in 1100 ml of tetrahydrofuran and the reaction mixture is stirred at −78° C. for 2 hours. 66 g of 4,4-dimethylcyclohexane dissolved in 210 ml of tetrahydrofuran are added at this same temperature and the reaction mixture is stirred for 1 hour at −78° C. The reaction mixture is hydrolysed by addition of crushed ice. The organic phase is separated out after settling of the phases has taken place, it is dried over sodium sulphate and the solvents are evaporated off under reduced pressure. The compound obtained is recrystallized from 500 ml of n-hexane; m.p.=88° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06482986B1 |
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| 出典データセット | uspto-grants-2002_11 |
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| ORD ID | ord-44b86795716e4ad79350c88828f2e8e9 |
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| 出典メモ | uspto-grants-2002_11 |
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