関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cyclopentylhydrazine hydrochloride | HCID 212349 | — |
| 反応物 | 1-(4-Bromo-2-nitrophenyl)butane-1,3-dione | HCID 86694314 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 5-(4-bromo-2-nitrophenyl)-1-cyclopentyl-3-methyl-1H-pyrazole | HCID 86694313 | 62.9% |
反応手順
Under a nitrogen atmosphere, to a solution of 1.0 g of 1-(4-bromo-2-nitrophenyl)butane-1,3-dione in 10 ml of acetic acid was added 501 mg of cyclopentylhydrazine hydrochloride, followed by stirring at 100° C. for 1 hour and 30 minutes. The reaction mixture was concentrated, and to the obtained residue was added ethyl acetate. The solution was washed with a saturated aqueous sodium hydrogen carbonate solution 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 (chloroform/methanol) to obtain 770 mg of 5-(4-bromo-2-nitrophenyl)-1-cyclopentyl-3-methyl-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-a380d65bfdde4e3f8411965e030bc974 |
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| 出典メモ | uspto-grants-2014_09 |
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