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Hydrochloric Acid → N-phenyl-5-nitro-2-thienylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Thiophene, 2-nitro- | HCID 11866 | — |
| 反応物 | Benzenesulfenamide, N-phenyl- | HCID 315504 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-phenyl-2-nitro-3-thienylamine | HCID 13039998 | 15% |
| 生成物 | N-phenyl-5-nitro-2-thienylamine | HCID 19783600 | 42% |
反応手順
2.9 g of 2-nitrothiophene and 4 g of N-phenylbenzenesulphenamide, dissolved in 10 ml of dimethylformamide, are added dropwise to a stirred solution of 6 g of potassium tert.-butylate in 60 ml of dimethylformamide, while the temperature is kept at about -20° C. The mixture is stirred for a further 15 minutes; then an excess of dilute hydrochloric acid is added to the mixture, after which it is treated in the same way as described in Example 1. The crude product is separated by column chromatography; N-phenyl-5-nitro-2-thienylamine (melting point 186° C., yield 1.8 g, 42%) and N-phenyl-2-nitro-3-thienylamine (melting point 105° C., yield 0.7 g, 15%) are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05262539 |
| 出典データセット | uspto-grants-1993_11 |
| ORD ID | ord-163f67be382447bcb75b33046858f377 |
| 出典メモ | uspto-grants-1993_11 |