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 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 2-Bromo-4-nitro-4'-(N,N-diethylamino)azobenzene | HCID 23341444 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Butyl Acetate | HCID 31272 | — |
| 生成物 | 2-((4-(Diethylamino)phenyl)azo)-5-nitrobenzonitrile | HCID 3015822 | 75% |
反応手順
2-Bromo-4-nitro-4'-(N,N-diethylamino)azobenzene (1.9 parts), copper (I) iodide (0.95 parts), anhydrous sodium acetate (1.2 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 temperatures is maintained at 110° C. for 31/2 hours when reaction is adjudged complete by thin layer chromatography. The solvent is removed at 80° C. under reduced pressure and the residue is slurried in water (250 parts), collected and dried. 2-Cyano-4-nitro-4'-(N,N-diethylamino)azobenzene is obtained in 75% yield and requires no purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04222935 |
|---|
| 出典データセット | uspto-grants-1980_09 |
|---|
| ORD ID | ord-99c02245faa74ee4a81ad4cfc92bd3be |
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| 出典メモ | uspto-grants-1980_09 |
|---|
