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Ethanol → 8-Hydroxyjulolidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 1-Bromo-3-chloropropane | HCID 8006 | — |
| 反応物 | 3-Aminophenol | HCID 11568 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | 8-Hydroxyjulolidine | HCID 170474 | 35% |
反応手順
m-Aminophenol (1.1 g, 10 mmol), 1-bromo-3-chloropropane (4.8 g, 3 ml, 30 mmol) and ethanol (10 ml) were placed in a 100 ml two-necked round-bottomed flask. The mixture was heated and refluxed for 11 hours, during which an NaHCO3 aqueous solution (2.0 g, 20 ml, 23 mmol) was added. The mixture was further heated and refluxed for 37 hours. The solvent was removed by distillation under reduced pressure. The resulting crude product was extracted with hexane by a solid-liquid continuous extraction to give 8-hydroxyjulolidine (661 mg) in 35% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06433176B1 |
| 出典データセット | uspto-grants-2002_08 |
| ORD ID | ord-e3674b5e94114bc79142154a9fbf5eb4 |
| 出典メモ | uspto-grants-2002_08 |