関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Potassium Cyanide | HCID 9032 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 1-Cyclopropylpropan-2-one | HCID 537025 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-Amino-3-cyclopropyl-2-methyl-propionitrile | HCID 84716049 | 63% |
反応手順
To a solution of 1-cyclopropyl-propan-2-one (1.0 g, 10.2 mmol; CAN 4160-75-2) and aqueous ammonia (25% in water, 15 mL) in EtOH (10 mL) was added ammonium chloride (1.63 g, 30.61 mmol). The reaction mixture was stirred at ambient temperature for 1 hour. To this was added potassium cyanide (900 mg, 15.3 mmol) portion wise and the reaction mixture was stirred at ambient temperature for 12 h. Ice water (50 mL) was added and the mixture was extracted with ethyl acetate (3×50 mL). The organic phases were washed with ice water, combined, dried with Na2SO4 and concentrated in vacuo to give the title compound (0.8 g, 63%) as yellow oil. 1H-NMR (DMSO, 400 MHz): 0.14-0.16 (d, 6.4 Hz, 2H); 0.45-0.49 (d, 6.4 Hz, 2H); 0.78-0.85 (m, 1H); 1.39 (s, 3H); 1.46-1.51 (m, 1H), 1.53-1.63 (m, 1H); 2.52 (br s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09290451B2 |
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| 出典データセット | uspto-grants-2016_03 |
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| ORD ID | ord-600cf380d7fe4a6b9c62205ec1488999 |
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| 出典メモ | uspto-grants-2016_03 |
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