関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Chloro-N,N-dimethylethylamine | HCID 7901 | — |
| 反応物 | Lithium hydride | HCID 62714 | — |
| 反応物 | 2-(2-Phenylethyl)phenol | HCID 2749041 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Ethanamine, N,N-dimethyl-2-(2-(2-phenylethyl)phenoxy)-, hydrochloride | HCID 3055342 | 95.1% |
反応手順
To a suspension of 1.0 g of lithium hydride in 30 ml of toluene was added dropwise a solution of 3.96 g of 2-hydroxybibenzyl in 30 ml of toluene at room temperature over 5 minutes. The mixture was heated under reflux for 30 minutes, a solution of 6.45 g of 2-chloro-N,N-dimethylethylamine in 20 ml of toluene added dropwise under reflux over 5 minutes and then reflux was continued for an additional 2 hours. The reaction mixture was cooled to room temperature, and to this was added 50 ml of water. The toluene layer was separated, washed twice with water, dried over anhydrous sodium sulfate and then the toluene distilled off in vacuo. The residue was dissolved in ethyl ether, and then 20% ethanolic hydrogen chloride solution was added. The resulting precipitate was collected by filtration and recrystallized from ethanol-ether to give 5.81 g (95% yield) of 2-(2-dimethylaminoethoxy)bibenzyl hydrochloride, m. p. 172°-173° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04220603 |
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| 出典データセット | uspto-grants-1980_09 |
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| ORD ID | ord-63c4908e65fa4f2d8afcdfd079ecea39 |
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| 出典メモ | uspto-grants-1980_09 |
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