참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | 5-(3,3-Difluoroazetidin-1-yl)-4-(2,2,2-trifluoroethoxy)picolinonitrile | HCID 90203299 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 5-(3,3-Difluoroazetidin-1-yl)-4-(2,2,2-trifluoroethoxy)picolinic acid | HCID 90204045 | 55% |
반응 단계
To a solution of 5-(3,3-difluoroazetidin-1-yl)-4-(2,2,2-trifluoroethoxy)pyridine-2-carbonitrile (example 223a, 680 mg, 2.32 mmol) in EtOH (8 ml) in a schlenk tube was added a 4M aqueous solution of potassium hydroxide (651 mg, 11.6 mmol). The reaction mixture was stirred at 105° C. for 2 hours. The reaction mixture was diluted with ethyl acetate and poured in a separatory funnel. The organic phase was extracted with a 1M aqueous solution of hydrochloric acid. The organic phase was collected and the aqueous phase was back-extracted with ethyl acetate. Combined organic phases were dried over sodium sulfate and evaporated down to dryness to yield the title compound (397 mg, 55%) as a crude solid which was used without any purification. MS (ESI, m/z): 311.2 (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-e9ca24f14cdb4fedb64964d2b06317f0 |
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| 출처 메모 | uspto-grants-2016_08 |
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