関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Benzenecarboximidamide, 4-hydroxy-, hydrochloride (1:1) | HCID 217124 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 4-Amidino-2-nitrophenol hydrochloride | HCID 136352310 | — |
反応手順
4-Amidinophenol hydrochloride (1.0 g, 5.8 mmol) was dissolved in concentrated sulfuric acid (2.5 mL), and concentrated nitric acid (0.38 mL) was added at −15° C. The reaction mixture was stirred for 1 hour while maintaining the temperature of the reaction mixture at −15° C. to −2° C., and slowly added to ice water. The mixture was neutralized by slowly adding sodium hydrogen carbonate, and the precipitated orange solid was collected by filtration. The solid was washed with water and acetone, and suspended in methanol. 4N Hydrochloric acid/dioxane was added to dissolve the solid. Diisopropyl ether was added to the solution, and the precipitated solid was collected by filtration. The solid was washed with diisopropyl ether and dried to give the title compound (0.98 g) as a pale-yellow powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09115107B2 |
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| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-713ed981356d495f835d656758eebf93 |
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| 出典メモ | uspto-grants-2015_08 |
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