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2-Aminophenol → 4-fluoro-N-(2-hydroxyphenyl)-3-nitrobenzanilide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Aminophenol | HCID 5801 | — |
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Fluoro-3-nitrobenzoic acid | HCID 67987 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-fluoro-N-(2-hydroxyphenyl)-3-nitrobenzanilide | HCID 67497934 | 68% |
反応手順
To a solution of 4-fluoro-3-nitrobenzoic acid (2.00 g, 10.8 mmol) in chloroform (40 mL) was added 2-aminophenol (1.18 g, 10.8 mmol), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (2.17 g, 11.3 mmol), and triethylamine (1.15 g, 11.3 mmol), and this was stirred at room temperature for 2.5 hours. After the reaction was complete, this was diluted by adding ethyl acetate, and this was washed with water, 1N hydrochloric acid, and saturated aqueous sodium hydrogen carbonate. The organic layer obtained was dried over anhydrous sodium sulfate, after which it was filtered and concentrated to yield the title compound (2.02 g, 68% yield) as orange crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08829035B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-e51a015c6d30428c8a4b915518a238cb |
| 出典メモ | uspto-grants-2014_09 |