関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitrone | HCID 6350 | — |
| 反応物 | Nitrobenzene | HCID 7416 | — |
| 反応物 | 2,6-Lutidine | HCID 7937 | — |
| 反応物 | 4-[(2,4-dibromo-6-methylphenyl)diazenyl]-N,N-diethylaniline | HCID 12525527 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 生成物 | 4-(2'-cyano-4'-bromo-6'-methylphenylazo)-N,N-diethylaniline | HCID 20347455 | 15.1% |
反応手順
A stirred mixture of 4-(2',4'-dibromo-6'-methylphenylazo)-N,N-diethylaniline (4.25 parts), copper (I) iodide (2.0 parts), formaldoxime trimer (1.75 parts), 2,6-lutidine (2.15 parts), and nitrobenzene (150 parts) was heated to 95° C. for 6 hours when thin layer chromatography showed reaction to be complete. The mixture was cooled, filtered and the nitrobenzene was removed by steam distillation. Crystallisation of the solid product from ethanol gave 4-(2'-cyano-4'-bromo-6'-methylphenylazo)-N,N-diethylaniline (Found: C, 58.2; H, 5.4; Br, 21.7; N, 15.2. C18H19BrN4 requires C, 58.2; H, 5.15; Br, 21.55; N, 15.1%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04192800 |
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| 出典データセット | uspto-grants-1980_03 |
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| ORD ID | ord-54d85bb108784b8bbeaa97feaa27ce35 |
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| 出典メモ | uspto-grants-1980_03 |
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