関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-(Dimethylamino)-2-methylpropanol | HCID 23435 | — |
| 反応物 | N,N-Dimethylaminoethyl chloride hydrochloride | HCID 11636816 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-[2-(dimethylamino)ethoxy]-N,N,2-trimethylpropane-2-amine | HCID 86657614 | 27% |
反応手順
To toluene (100 ml), sodium hydroxide (16.7 g, 418 mmol) and 2-dimethylamino-2-methyl-1-propanol (23.4 g, 200 mmol) were added and the mixture was heated at reflux for 2 hours. After cooling to 70° C., β-dimethylaminoethyl chloride hydrochloride (28.8 g, 200 mmol) was added. Then, the mixture was heated at reflux for 5.5 hours. After cooling to room temperature, insolubles were separated by filtration and the organic phase was concentrated under reduced pressure. The residue was distilled under reduced pressure to obtain 10.3 g (in a yield of 27%) of the objective compound as a colorless liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08871970B2 |
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| 出典データセット | uspto-grants-2014_10 |
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| ORD ID | ord-dc8c5e0dd9064b429536880dde457406 |
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| 出典メモ | uspto-grants-2014_10 |
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