関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,4-Dinitroaniline | HCID 7321 | — |
| 反応物 | 3,5-Dinitrobenzoyl chloride | HCID 7432 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 2',3,4',5-Tetranitrobenzanilide | HCID 298942 | 8.1% |
反応手順
2,4-dinitroaniline (18.05 g), triethylamine (12.97 g) and benzene (750 ml) were placed in a reaction vessel and stirred under the nitrogen atmosphere. To the reaction mixture, 3,5-dinitrobenzoyl chloride (25.00 g) was added and refluxed under heating for 6 hours. The reaction mixture was filtered in hot state and the filtrate was cooled to deposit crystals of 2',3,4',5-tetranitrobenzanilide which was collected by filtration. The product of 2',3,4',5-tetranitrobenzanilide (3.00 g) thus obtained, platinum/carbon (5%) (0.18 g) and dioxane (85 ml) were placed in a pressurized vessel and allowed to react under the hydrogen pressure of 1 to 3 kg/cm2 at 80° C. for 10 hours. After cooling, the catalyst was removed by filtration and dioxane was distilled off under the reduced pressure to obtain powder of 2',3,4',5-tetraaminobenzanilide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04761234 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-6556d3199ab54b82bec6064b8264157e |
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| 出典メモ | uspto-grants-1988_08 |
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