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Water → 3-(5-Nitrofuran-2-yl)-1-phenyl-1H-pyrazole-4-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Nitrosylsulfuric acid | HCID 82157 | — |
| 反応物 | 3-(5-Nitrofuran-2-yl)-1-phenyl-1H-pyrazole-4-carboxamide | HCID 20326123 | — |
| 溶媒 | Phosphoric Acid | HCID 1004 | — |
| 生成物 | 3-(5-Nitrofuran-2-yl)-1-phenyl-1H-pyrazole-4-carboxylic acid | HCID 20325964 | 98% |
反応手順
Add 36 g of 98% nitrosylsulfuric acid (under cooling with ice) dropwise to a suspension of 50 g 3-(5-nitro-2-furyl)-1-phenylpyrazole-4-carboxamide in 830 ml of 89% orthophosphoric acid, whereupon the temperature rises from 0° C to 35° C. Stir the resulting reaction mixture for 18 hours at room temperature and pour the produced solution onto 5 kg of ice and water. Separate the formed precipitate and wash it with water until it is no longer acid to obtain a 98% yield of 3-(5-nitro-2-furyl)-1-phenylpyrazole-4-carboxylic acid [m.p. 264° to 265.5° C (with decomposition) from dioxane].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04093812 |
| 出典データセット | uspto-grants-1978_06 |
| ORD ID | ord-d72558aeda8b436aa12c823a1e0915d3 |
| 出典メモ | uspto-grants-1978_06 |