関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formamide | HCID 713 | — |
| 反応物 | Propionic anhydride | HCID 31263 | — |
| 反応物 | Acetamide, N-[2-[2-(2-bromo-4,6-dinitrophenyl)diazenyl]-5-(diethylamino)phenyl]- | HCID 104287 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 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 | 83.5% |
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 sodium acetate (1.2 parts), formamide (1.8 parts), propionic anhydride (2.6 parts) and n-butyl acetate (44 parts) are mixed together are heated, with stirring, to 110° C. during 15 minutes. The temperature is maintained for 30 minutes when reaction is adjudged complete by thin layer chromatography. 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 83.5% 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-bd6608fb4bfe4cc9af4f818a4bca50c8 |
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| 出典メモ | uspto-grants-1980_09 |
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