関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | 4-Fluoroaniline | HCID 9731 | — |
| 反応物 | Diethyl isopropylidenemalonate | HCID 81255 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ethyl 2-(4-fluorophenylcarbamoyl)-3-methylbut-2-enoate | HCID 66767015 | 39% |
反応手順
To a solution of 4-fluoroaniline (2 g, 18 mmol) in diethyl isopropylidenemalonate (10 g, 50 mmol) is added 1H-imidazole (0.25 g, 3.67 mmol). The reaction mixture is stirred at 200° C. under N2 for 3 hours. After the reaction is cooled, silica gel is added. The mixture is loaded onto a silica gel column, and eluted first with PE and then PE:EtOAc (3:1) to give the product (1.85 g, 39% yield). MS (m/z): 266.1 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08030302B2 |
|---|
| 出典データセット | uspto-grants-2011_10 |
|---|
| ORD ID | ord-93ee3a44f7fd409fb10f6c02f3b7b135 |
|---|
| 出典メモ | uspto-grants-2011_10 |
|---|
