関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 2-Methyl-2-(morpholin-4-yl)propanenitrile | HCID 2423784 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Methyl-2-morpholin-4-ylpropanamide | HCID 7471956 | — |
反応手順
272 ml of concentrated sulfuric acid are slowly added, with stirring, to 57.9 g of 2-methyl-2-morpholino-propionitrile (exothermic reaction). After the addition of 43 ml of water, the mixture is stirred for 2 hours at 100°-110° C. The reaction mixture is cooled to 50° C. and added dropwise at 0° C. to a solution of 846 ml of 20% ammonia in 242 ml of water. The mixture is then extracted repeatedly with dichloromethane. The organic phases are washed with saturated sodium chloride solution and with sodium sulfate. The crude title compound is obtained from the concentrated filtrate: 1H NMR (CDCl3), δ(ppm) =7.08 (1 H, bs), 5.38 (1H, bs), 3.72 (4H, m), 2.53 (4H, m), 1.22 (6H, s)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05646143 |
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| 出典データセット | uspto-grants-1997_07 |
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| ORD ID | ord-6b5f3c012223497693241617d5cbcdf6 |
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| 出典メモ | uspto-grants-1997_07 |
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