참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Sodium Cyanide | HCID 8929 | — |
| 반응물 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | 1-Cyclopropylpropan-2-one | HCID 537025 | — |
| 생성물 | 2-Amino-3-cyclopropyl-2-methyl-propionitrile | HCID 84716049 | 177.2% |
반응 단계
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+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09409866B2 |
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| 출처 데이터셋 | uspto-grants-2016_08 |
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| ORD ID | ord-cbce99c91cb54737a1dfdb27616d092c |
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| 출처 메모 | uspto-grants-2016_08 |
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