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4-Nitrophthalimide → (5-Nitro-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-acetic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Nitrophthalimide | HCID 6969 | — |
| 反応物 | Ethyl bromoacetate | HCID 7748 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | (5-Nitro-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-acetic acid ethyl ester | HCID 784823 | 89.8% |
反応手順
A mixture of 4-nitrophthalimide (82.54 g, 0.43 mol), ethyl bromoacetate (78.92 g, 0.47 mol) and potassium carbonate (130.6 g, 0.94 mol), and acetone (1.5 l) was refluxed for eighteen hours before it was cooled to room temperature, filtered and concentrated in vacuo. The residue was partitioned between dichloromethane and water. The organic layer was dried over anhydrous sodium sulfate and concentrated in vacuo to give the title compound as a yellow solid (107.39 g): MS: (+) m/z 279.25 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08759373B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-7bff02a827b248418e5164c7a19d1b7f |
| 出典メモ | uspto-grants-2014_06 |