참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 반응물 | Benzamidine, hydrochloride | HCID 80289 | — |
| 반응물 | Ethyl 3-acetamido-2-oxobutanoate | HCID 22245807 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | N-[1-(5-Oxo-3-phenyl-4,5-dihydro-1,2,4-triazin-6-yl)ethyl]acetamide | HCID 136024651 | — |
반응 단계
48 g (306 mmol) of benzenecarboximidamide hydrochloride were dissolved in 1.2 l ethanol, and 16.4 ml (337 mmol) of hydrazine hydrate were added. The mixture was stirred at 45° C. for 3 h. 86 g (459 mmol) of ethyl 3-acetamido-2-oxobutanoate (Example 13A), dissolved in 600 ml of ethanol, were added dropwise. The mixture was stirred at 80° C. for another 6 h and at RT for another 12 h. The reaction mixture was chromatographed on silica gel (mobile phase dichloromethane/methanol 20:1). This gave 23.2 g (26% of theory) of the product as a solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08476267B2 |
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| 출처 데이터셋 | uspto-grants-2013_07 |
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| ORD ID | ord-f2284a1a3f3d4da7a9ef486a2b64eac9 |
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| 출처 메모 | uspto-grants-2013_07 |
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