関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formamide | HCID 713 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Acetamide, N-[2-[2-(2-bromo-4,6-dinitrophenyl)diazenyl]-5-(diethylamino)phenyl]- | HCID 104287 | — |
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Butyl Acetate | HCID 31272 | — |
| 生成物 | Acetamide, N-(2-(2-(2-cyano-4,6-dinitrophenyl)diazenyl)-5-(diethylamino)phenyl)- | HCID 90383 | 95% |
反応手順
2-Bromo-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino) azobenzene (2.4 parts), copper (I) iodide (0.95 parts), anhydrous potassium acetate (1.5 parts), formamide (1.8 parts), acetic anhydride (2.0 parts) and n-butyl acetate (44 parts) are mixed together and heated, with stirring, to 110° C. during 15 minutes. The temperature is maintained at 110° C. for 2 hours when reaction is complete. The mixture is cooled to room temperature and poured into petroleum ether (boiling range 60-80° C.) (400 parts). The precipitate is collected, washed with petroleum ether (100 parts) and dried. 2-Cyano-4,6-dinitro-2'-acetylamino-4'-(N,N-diethylamino)azobenzene is obtained in 95% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04222935 |
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| 出典データセット | uspto-grants-1980_09 |
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| ORD ID | ord-93bd652589b648a7801ab04648adafb1 |
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| 出典メモ | uspto-grants-1980_09 |
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