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2-Chlorophenol → 3-(Diethylamino)phenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Chlorophenol | HCID 7245 | — |
| 反応物 | Diethylamine | HCID 8021 | — |
| 反応物 | Sodium amide | HCID 24533 | — |
| 生成物 | 3-(Diethylamino)phenol | HCID 7062 | 76% |
反応手順
32.1 g (0.25 mol) of o-chlorophenol were slowly added dropwise under nitrogen to a mixture of 20.5 g (0.5 mol) of 95% by weight pure crystalline sodium amide and 750 ml of diethylamine. The reaction mixture was refluxed under nitrogen for 72 h with stirring. The workup comprised hydrolysis with 100 ml of saturated aqueous ammonium chloride solution, distillative removal of excess diethylamine, neutralization with dilute hydrochloric acid up to a pH of 7.5, extraction of the residue with a total of 600 ml of methylene chloride, drying over sodium sulfate and concentrating of the organic phase. Thereafter the crude oil thus obtained (46.3 g) was distilled, which yielded 31.5 g (76%) of 3-diethylaminophenol (purity>96% (GC)).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05486609 |
| 出典データセット | uspto-grants-1996_01 |
| ORD ID | ord-cc3170317df24e0da1d82fe75269e464 |
| 出典メモ | uspto-grants-1996_01 |