関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | 1,3-Benzodioxole, 5-nitro- | HCID 75798 | — |
| 生成物 | 5,6-Dinitro-1,3-benzodioxole | HCID 611325 | — |
反応手順
0.103 mol (17.2 g) of 4,5-methylenedioxy-1-nitrobenzene is added in small portions in the course of 15 minutes to a mixture, cooled to -5° C., consisting of 125 ml of nitric acid (d=1.50) and 125 ml of nitric acid (d=1.40), the temperature being maintained at between 0° and 5° C. 1 hour after the addition is complete, the reaction mixture is poured onto 1 kg of ice. The expected product precipitates. After being dried hot in the presence of phosphorus pentoxide, it melts at 99° C. (literature 98°-100° C.). It can optionally be recrystallized from 96° strength ethanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04749379 |
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| 出典データセット | uspto-grants-1988_06 |
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| ORD ID | ord-7a1e47a7683e4485b828e5fb555ebd67 |
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| 出典メモ | uspto-grants-1988_06 |
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