참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | 2,4-Difluorobenzene-1-thiol | HCID 2737073 | — |
| 반응물 | 2,6-Dichloropyridine-3-carbonitrile | HCID 12605538 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-Chloro-6-(2,4-difluorophenylthio)nicotinonitrile | HCID 86680563 | 66% |
반응 단계
A solution of 362 mg (1.05 eq) of potassium hydroxide in 10 mL of ethanol is added, under nitrogen, to a solution of 698 μL (6.16 mmol) of 2,4-difluorobenzenethiol in 30 mL of ethanol. The reaction medium is stirred at room temperature for 15 minutes and then cooled in ice before adding a solution of 1.015 g (0.95 eq) of 2,6-dichloronicotinonitrile in 30 mL of ethanol. The reaction medium is stirred for 2 hours at 0-5° C. 63 mL of a 0.1N HCl solution is added to stop the reaction. Water is added and the producted is extracted with ethyl acetate. The organic phase is dried on anhydrous magnesium sulfate, filtered and evaporated. The residue is purified by silica gel chromatography (eluent: cyclohexane/ethyl acetate 94:6) to yield 1.09 g (66%) of 2-chloro-6-(2,4-difluorophenylthio)-nicotinonitrile in the form of a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08883821B2 |
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| 출처 데이터셋 | uspto-grants-2014_11 |
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| ORD ID | ord-3bc7bc0b9b2d446d9bd68515daf4eecd |
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| 출처 메모 | uspto-grants-2014_11 |
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