참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Cyclopentylhydrazine hydrochloride | HCID 212349 | — |
| 반응물 | Water ethylacetate | HCID 22728543 | — |
| 반응물 | HCID 86694307 | HCID 86694307 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 5-(4-bromo-2-nitrophenyl)-1-cyclopentyl-1H-pyrazole | HCID 86694306 | 72.7% |
반응 단계
Under a nitrogen atmosphere, to a solution of 1.15 g of (2E)-1-(4-bromo-2-nitrophenyl)-3-(dimethylamino)prop-2-en-1-one in 9.2 mL of acetic acid was added 1.05 g of cyclopentylhydrazine hydrochloride, followed by stirring at room temperature for 60 hours. The reaction mixture was poured into a mixture of water/ethyl acetate, followed by adjusting to pH 10 with a 6 M aqueous sodium hydroxide solution. The aqueous layer was separated, and then the organic layer was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and then the residue was purified by silica gel column chromatography (n-hexane/ethyl acetate) to obtain 940 mg of 5-(4-bromo-2-nitrophenyl)-1-cyclopentyl-1H-pyrazole.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08822448B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-cf396f515aa44bb389aea08b1452c5fb |
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| 출처 메모 | uspto-grants-2014_09 |
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