関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Hydrazinoethanol | HCID 8017 | — |
| 反応物 | 3,3-Dimethoxy-2-hydroxyiminopropionitrile | HCID 71361562 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-Amino-1-(2-hydroxyethyl)-4-nitrosopyrazole hydrochloride | HCID 18426880 | 94% |
反応手順
To a flask having an inner volume of 25 ml and equipped with a stirring device, a thermometer and a reflux condenser were charged 1.47 g (10.0 mmol) of 3,3-dimethoxy-2-hydroxyiminopropionitrile with a purity of 98.1% by weight synthesized in the same manner as in Example 1, 0.84 g (10.5 mmol) of 2-hydroxyethylhydrazine with a purity of 95% by weight, 10 ml of methanol and 1.5 ml (18.0 mmol) of conc. hydrochloric acid, and the mixture was reacted under reflux (67° C.) for 1.5 hours. After completion of the reaction, when the reaction mixture was analyzed by high performance liquid chromatography (absolute calibration curve method), it was found that 1.81 g of 5-amino-1-(2-hydroxyethyl)-4-nitrosopyrazole hydrochloride (Reaction yield: 93.8%) had been formed.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07227032B2 |
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| 出典データセット | uspto-grants-2007_06 |
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| ORD ID | ord-5181e8ae4bda4f58be10c7f24ccf6c1a |
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| 出典メモ | uspto-grants-2007_06 |
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