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Ethyl Acetate → 5-(Trifluoromethoxy)-1H-indole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Sodium Sulfate | HCID 24436 | — |
| 反応物 | 5-(trifluoromethoxy)-2,3-dihydro-1H-indole-2,3-dione | HCID 2732752 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-(Trifluoromethoxy)-1H-indole | HCID 17989050 | 23.3% |
反応手順
Lithium aluminum hydride (10.4 mL, 1M in THF, 10.4 mmol) was added to a solution of 5-trifluoromethoxyisatin (0.8 g, 3.45 mmol) in THF at room temperature and the mixture was refluxed overnight. The reaction mixture was cooled, and Na2SO4 10H2O was added very carefully portionwise, followed by ethyl acetate. The reaction mixture was then filtered, and the filtrate was evaporated. The residual oil was purifed by column chromatography with ethyl acetate in hexanes (2:98) to yield 5-trifluoromethoxy-1H-indole (0.162 g, 23%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06133287 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-db4b385c5414493e9da7264059cc4606 |
| 出典メモ | uspto-grants-2000_10 |