関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Semicarbazide hydrochloride | HCID 11236 | — |
| 反応物 | alpha-Acetyl-4-phenylthiophenylacetonitrile | HCID 54503700 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Amino-5-methyl-4-(4-phenylthiophenyl)pyrazole | HCID 19934711 | 91.4% |
反応手順
A mixture of 520 mg of α-acetyl-4-phenylthiophenylacetonitrile, 217 mg of semicarbazide hydrochloride, 15 ml of methanol and 3 ml of water was stirred at 0° C. for 10 minutes. Removing the ice bath, 40 hours later, the mixture was stirred at room temperature for 1 hour while keeping the pH at 9 to 10 by using aqueous solution of 2N sodium hydroxide. Adding 50 ml of water, the mixture was stirred for 30 minutes in ice-cooling, and the precipitate was filtered. It was directly added to the mixed solution of 5 ml of aqueous solution of 2N sodium hydroxide and 50 ml of methanol, and the mixture was stirred for 4 hours at room temperature, and then 80 ml of water was added, and the mixture was stirred for 30 minutes in ice-cooling, then the precipitate was filtered, Washed in water and dried, thereby obtaining 500 mg of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05420128 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-0e139b0d9c6a49fbb305c957012777d5 |
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| 出典メモ | uspto-grants-1995_05 |
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