関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Chloro-2-(diethylamine)ethane hydrochloride | HCID 13363 | — |
| 反応物 | HCID 178526976 | HCID 178526976 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | Diethyl[2-(4-nitrophenoxy)ethyl]amine | HCID 88294 | 79.5% |
反応手順
4-Nitrophenoxy sodium dihydrate (29.39 g), 2-(diethylamino)ethylchloride hydrochloride (25.60 g), potassium carbonate (30.17 g) and water (60 ml) were added into xylene (100 ml) and the mixture was heat-refluxed for 2 hours while mixing and continuously removing water by azeotropic distillation. After reaction, insolubles were removed by filtration. Filtrate was added with ethyl acetate (100 ml) and extracted 3 times with 1N HCl (100 ml). Aqueous layer was adjusted to pH 10 with 1N sodium hydroxide and oily substance separated was extracted 3 times with ethyl acetate (100 ml). Ethyl acetate solution was dehydrated with anhydrous magnesium sulfate and concentrated to obtain N,N-diethyl-2-(4-nitrophenoxy)ethylamine (28.19 g) as color-less oily substance.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06300368B1 |
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| 出典データセット | uspto-grants-2001_10 |
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| ORD ID | ord-5642302a26bc4e7a83e80cc162e8c81c |
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| 出典メモ | uspto-grants-2001_10 |
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