関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Sodium Cyanide | HCID 8929 | — |
| 反応物 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 1-Cyclopropylpropan-2-one | HCID 537025 | — |
| 生成物 | 2-Amino-3-cyclopropyl-2-methyl-propionitrile | HCID 84716049 | 177.2% |
反応手順
To a round bottom flask equipped with a condenser was added magnesium sulfate (4.33 g, 35.9 mmol), sodium cyanide (3.52 g, 71.9 mmol) and ammonium chloride (1.92 g, 35.9 mmol). The solids were slurried in a 7.0M solution of ammonia in methanol (30.8 ml, 216 mmol) at room temperature. To the resulting suspension was added 1-cyclopropylpropan-2-one (CAN 4160-75-2, 8.3 g, 71.9 mmol) in one portion. The reaction mixture was stirred at room temperature for 4 hours. The solvents were removed under reduced pressure. The resulting slurry of the inorganic salts and product were diluted with tert-butylmethylether and solvent removed at reduced pressure. This process was repeated three times before the resulting suspension was filtered to remove the inorganic salts. The filtrate was then evaporated down to dryness to yield the crude product (7.9 g, 89%) as a yellow oil. MS (ESI, m/z): 125.3 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09409866B2 |
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| 出典データセット | uspto-grants-2016_08 |
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| ORD ID | ord-cbce99c91cb54737a1dfdb27616d092c |
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| 出典メモ | uspto-grants-2016_08 |
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