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Aluminium lithium hydride → 5-methyl-3-(pyrrolidin-3-yl)-1H-indole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | 3-(5-methyl-1H-indol-3-yl)pyrrolidine-2,5-dione | HCID 67036471 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-methyl-3-(pyrrolidin-3-yl)-1H-indole | HCID 54857136 | — |
反応手順
Lithium aluminum hydride (7.9 g, 200 mmol) in dry THF (380 mL) was stirred for 20 min. at RT under nitrogen atmosphere. 3-(5-Methyl-1H-indol-3-yl) pyrrolidine-2,5-dione (9.5 g, 41 mmol) was added portionwise and the reaction mixture was heated to reflux overnight. The reaction mixture was cooled to RT, quenched with aqueous sodium sulfate, and filtered. The solid was rinsed with THF and the THF layer was dried over anhydrous sodium sulfate and evaporated under reduced pressure. The residue was purified by silica gel chromatography (25% MeOH/DCM/ammonia) to afford the title compound. Yield: 4.2 g, 49.2%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09271971B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-0a63783d039e4223ae006b1871f57cff |
| 出典メモ | uspto-grants-2016_03 |