関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetoacetate | HCID 8868 | — |
| 反応物 | Phenylhydrazine hydrochloride | HCID 60962 | — |
| 反応物 | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 5-methyl-1-phenyl-1H-pyrazole-4-carboxylate | HCID 96680 | 87.6% |
反応手順
A mixture of ethyl acetoacetate (1.5 g, 11.5 mmol) and dimethylformamide dimethyl acetal (1.68 mL, 12.7 mmol) was stirred at 120° C. for 2 hours. The reaction solution was cooled to room temperature, and a solution of phenyl hydrazine hydrochloride (1.67 g, 11.5 mmol) in ethanol (30 mL) was then added thereto. The obtained mixture was stirred at 80° C. for 2.5 hours. The reaction solution was cooled to room temperature, and it was then concentrated under reduced pressure. The residue was purified with a fractionation purification apparatus (Biotage, ethyl acetate:hexane=1:19-3:7), so as to obtain the title compound (2.32 g, 87%) in the form of a yellow oily product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09150563B2 |
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| 出典データセット | uspto-grants-2015_10 |
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| ORD ID | ord-ee94dc121ecc421b969e6bafb5fbde2b |
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| 出典メモ | uspto-grants-2015_10 |
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