関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Quintozene | HCID 6720 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | Pentachlorophenylhydrazine | HCID 20065461 | — |
反応手順
Pentachloronitrobenzene containing 5-10% hexaxchlorobenzene, (3.0 g, 10.1 mmole) was dissolved in dimethylsulphoxide (35 ml). Hydrazine hydrate (1.25 g, 25 mmole) was added dropwise with stirring at 25° C. A slight 4°-5° C. increase in temperature was recorded and the solution became red-brown. After approximately 20 minutes a white solid began to be precipitated. Stirring was continued for one hour after which time TLC (1:1 ethyl acetate: 60°-80° C. petrol) indicated that the reaction was complete. The mixture was poured into stirred water (200 ml) and the solid filtered off and dried at 50° C. overnight. The TLC and IR was identical to an authentic sample of pentachlorophenylhydrazine. Yield=2.27 g, 80%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05001262 |
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| 出典データセット | uspto-grants-1991_03 |
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| ORD ID | ord-22cfba713da1466a820183fa4ce93ade |
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| 出典メモ | uspto-grants-1991_03 |
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