化工社化工社 化学情報印刷レポート · 研究参考用
(+-)-3-Methyl-2,4(3H,5H)-furandione → 6-fluoro-3-(4-methoxy-5H-furan-2-ylidene)-1,3-dihydro-indol-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | (+-)-3-Methyl-2,4(3H,5H)-furandione | HCID 544553 | — |
| 反応物 | 6-fluoro-2,3-dihydro-1H-indol-2-one | HCID 3731013 | — |
| 反応物 | LiHMDS tetrahydrofuran | HCID 23714775 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 6-fluoro-3-(4-methoxy-5H-furan-2-ylidene)-1,3-dihydro-indol-2-one | HCID 69401606 | — |
反応手順
To a stirred solution of 6-fluorooxindole (2.6 g, 17.5 mmol) in anhydrous THF (30 mL) under nitrogen was added 1.0M LiHMDS/THF solution (35 mL, 35 mmol). The mixture was stirred at room temperature for 10 minutes. Methyl tetronate (1.0 g, 8.8 mmol) was added as one portion. After stirring at room temperature for 1 hour, the reaction was cooled to 0° C., and quenched with 2M HCl until pH=3. The mixture was stirred at room temperature for 2 more hours, and poured into 250 mL of water. The resulting precipitates were filtered, rinsed with water and dried in vacuum to give 6-fluoro-3-(4-methoxy-5H-furan-2-ylidene)-1,3-dihydro-indol-2-one as off-white solid. Yield: 840 mg, 38%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08865682B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-779849055d7d4a4683df490f9424c4be |
| 出典メモ | uspto-grants-2014_10 |