関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Phenol, 3,5-diamino-2,4,6-trinitro- | HCID 5249535 | — |
| 生成物 | Trinitrophloroglucinol | HCID 4555524 | 84% |
反応手順
Diaminopicric acid (0.100 g, 0.386 mmol) is suspended in water (6.85 ml) and a 50% aqueous solution of sodium hydroxide (0.65 ml,12.5 mmol) is added. The suspension is stirred for 0.5 hr in a heated water bath (98–100° C.) to produce an orange-red suspension which is cooled to 4° C. Addition of cold 12N hydrochloric acid (4 ml) produces a deep yellow suspension that is heated to solution. Cooling to 4° C. produces orange-yellow crystals (needles) that are collected, washed with cold 3N hydrochloric acid and dried to give trinitrophloroglucinol (0.085 g) in 84% yield. The IR spectrum for this material corresponds to that for known trinitrophloroglucinol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07057073B2 |
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| 出典データセット | uspto-grants-2006_06 |
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| ORD ID | ord-838ef8f22aae426493df74c337424133 |
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| 出典メモ | uspto-grants-2006_06 |
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