참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 3-Bromo-4-fluoroaniline | HCID 2779286 | — |
| 반응물 | N-Hydroxy-4-[(2-methoxyethyl)amino]-1,2,5-oxadiazole-3-carboximidoyl chloride | HCID 136330165 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 178495897 | HCID 178495897 | 98.6% |
반응 단계
N-Hydroxy-4-[(2-methoxyethyl)amino]-1,2,5-oxadiazole-3-carboximidoyl chloride (46.0 g, 0.208 mol) was mixed with water (300 mL). The mixture was heated to 60° C. 3-Bromo-4-fluoroaniline [Oakwood products, product #013091] (43.6 g, 0.229 mol) was added and stirred for 10 min. A warm sodium bicarbonate (26.3 g, 0.313 mol) solution (300 mL water) was added over 15 min. The reaction was stirred at 60° C. for 20 min. LCMS indicated reaction completion. The reaction solution was cooled to room temperature and extracted with ethyl acetate (2×300 mL). The combined ethyl acetate solution was dried over sodium sulfate and concentrated to give the desired product (76.7 g, 98%) as a crude brown solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08822511B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-8977d57a4e8342d2b25501863e7f168a |
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| 출처 메모 | uspto-grants-2014_09 |
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