関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-(o-Aminophenyl)-4-chloro-1-butanone hydrochloride | HCID 23293246 | — |
| 触媒 | Tributylmethylammonium chloride | HCID 91822 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (2-Aminophenyl)(cyclopropyl)methanone | HCID 10931741 | 70% |
反応手順
A solution of 0.30 g (1.3 mmol) of 1-(o-aminophenyl)-4-chloro-1-butanone hydrochloride in 3 mL of methylene chloride and 3 mL of ethylene dichloride is treated with 1.2 g (3 mmol) of 10% sodium hydroxide solution and 0.05 g (0.2 mmol) of 75% aqueous methyl tributylammonium chloride and heated to 50° C. for about 5 hours. After cooling to room temperature, the phases are separated. The aqueous layer is extracted with methylene chloride. The combined organic extracts are washed with water and concentrated in vacuo to give 0.14 g (70% yield) of o-aminophenyl cyclopropyl ketone (mp 46-48° C.). The product is identified by NMR and MS analyses.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06127576 |
|---|
| 出典データセット | uspto-grants-2000_10 |
|---|
| ORD ID | ord-c1e30ccef6c34666a0b9cc4091476cfe |
|---|
| 出典メモ | uspto-grants-2000_10 |
|---|