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Potassium Iodide → HCID 59257866、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Ethyl bromoacetate | HCID 7748 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | methyl (4-nitro-2,3-dihydro-1H-indol-3-yl)-acetate | HCID 10243182 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | HCID 59257866 | HCID 59257866 | — |
反応手順
To a solution of (±)-methyl (4-nitro-2,3-dihydro-1H-indol-3-yl)acetate from Step B (700 mg, 2.97 mmol), sodium carbonate (471 mg, 4.44 mmol), and potassium iodide (98 mg, 0.59 mmol) in acetone (15 mL) was added ethyl bromoacetate (9.9 mL, 88.9 mmol). The mixture was heated at reflux for 18 h, then cooled to ambient temperature and concentrated in vacuo. The residue was partitioned between H2O (15 mL) and EtOAc (2×40 mL) and the organic extracts were washed with brine, dried over Na2SO4, filtered, and concentrated in vacuo to a volume of 50 mL. Hexane was added to the EtOAc solution and a precipitate formed. The desired crystals were collected by vacuum filtration to give the title compound. MS: m/z=323 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07947677B2 |
| 出典データセット | uspto-grants-2011_05 |
| ORD ID | ord-e813476fa1df4e488706c7fa1b06cbaf |
| 出典メモ | uspto-grants-2011_05 |