関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Cyclopentylhydrazine hydrochloride | HCID 212349 | — |
| 反応物 | Water ethylacetate | HCID 22728543 | — |
| 反応物 | (2E)-1-(4-bromo-2-nitrophenyl)-3-(dimethylamino)prop-2-en-1-one | HCID 86694307 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 5-(4-bromo-2-nitrophenyl)-1-cyclopentyl-1H-pyrazole | HCID 86694306 | 72.7% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822448B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-cf396f515aa44bb389aea08b1452c5fb |
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| 出典メモ | uspto-grants-2014_09 |
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