참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 5-Bromo-2-(trifluoromethyl)isonicotinamide | HCID 68467662 | — |
| 용매 | Phosphorus oxychloride | HCID 24813 | — |
| 생성물 | 5-Bromo-2-(trifluoromethyl)isonicotinonitrile | HCID 56973315 | 94% |
반응 단계
To a 100 mL round bottom equipped with a stir bar, condenser and nitrogen inlet was charged 5.2 g (19.3 mmol) of 5-bromo-2-trifluoromethyl-isonicotinamide. The solid was diluted with 12 mL of phosphorus oxychloride. The mixture was heated at 70° C. for 3 hr. The mixture was cooled to ambient temperature and poured onto ice. The mixture was neutralized with the careful addition of 50% sodium hydroxide. The resulting off-white solid was collected by filtration, washed with water and dried in vacuo at 50° C. for 18 h. This afforded 4.5 g of 5-bromo-2-trifluoromethyl-isonicotinonitrile 1-1 as an off-white solid in a 94% yield. 1HNMR (CDCl3), δ, 9.03 (s, 1H), 7.91 (s, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08481738B2 |
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| 출처 데이터셋 | uspto-grants-2013_07 |
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| ORD ID | ord-743f7cb6eadc431083e86b8a9226cbf6 |
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| 출처 메모 | uspto-grants-2013_07 |
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