化工社化工社 化学情報印刷レポート · 研究参考用
Phenacyl bromide → Ethyl 2-acetyl-4-oxo-4-phenylbutanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phenacyl bromide | HCID 6259 | — |
| 反応物 | Ethyl Acetoacetate | HCID 8868 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl 2-acetyl-4-oxo-4-phenylbutanoate | HCID 312893 | 99.6% |
反応手順
To a solution of ethyl acetoacetate (10 g, 76.8 mmol) in tetrahydrofuran (50 ml) at 0° C. was added sodium hydride (4 g, 60% in mineral oil, 100 mmol) portionly. The reaction mixture was stirred for minutes, and 2-bromoacetophenone (16.8 g, 84.5 mmol) in tetrahydrofuran (20 ml) was added dropwisely. After warming the mixture to room temperature, it was stirred for 4 hours. The resulting solution was quenched with water and normal work-up accomplished with diethyl ether. The organic layer was dried with MgSO4, and purified by silica gel column chromatography (EtOAc:Hx=1:5) to produce desired compound (19 g, 98%) as light yellow color oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08895558B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-8412866a79de47c7b3611c0634a6a7f6 |
| 出典メモ | uspto-grants-2014_11 |