참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Ethylhydrazine | HCID 29062 | — |
| 반응물 | 4-Methoxy-3-oxobutanenitrile | HCID 23091966 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 1-ethyl-3-[(methyloxy)methyl]-1H-pyrazol-5-amine | HCID 57516908 | 55.8% |
반응 단계
To a 25 mL round bottom was added 4-(methyloxy)-3-oxobutanenitrile (500 mg, 4.42 mmol), ethyl hydrazine (655 mg, 4.42 mmol), and 2 M HCl (2.210 mL, 4.42 mmol) in ethanol (10 mL). The reaction mixture was stirred at the room temperature overnight. The reaction mixture was then evaporated and pardoned between 20 mL of ethyl acetate and 20 mL of 1 M Na2CO3. The organic layer was washed with brine, filtered and evaporated to obtain 1-ethyl-3-[(methyloxy)methyl]-1H-pyrazol-5-amine (450 mg, 2.465 mmol, 55.8% yield) as a yellow oil. The product was used in the next step without further purification. LCMS (M+H)+=156.1; 1H NMR (400 MHz, DMSO-d6) ppm 1.20 (t, J=7.20 Hz, 3 H) 3.19 (s, 3 H) 3.82 (q, J=7.33 Hz, 2 H) 4.11 (s, 2 H) 5.11 (s, 2 H) 5.22 (s, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09446034B2 |
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| 출처 데이터셋 | uspto-grants-2016_09 |
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| ORD ID | ord-e56584f606ac4cb2a9a9ca840156619c |
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| 출처 메모 | uspto-grants-2016_09 |
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