関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | 5-Bromo-2-(pyrrolidine-1-carbonyl)-1H-indole | HCID 47154657 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-bromo-2-pyrrolidin-1-ylmethyl-1H-indole | HCID 66670945 | — |
反応手順
To a suspension of (5-bromo-1H-indol-2-yl)-pyrrolidin-1-yl-methanone (0.53 g, 1.8 mmol) in THF (50 mL) at 0° C. was slowly added lithium aluminum hydride (0.20 g, 5.4 mmol). The mixture was stirred under nitrogen at 0° C. for a while and the cooling bath was allowed to warm to room temperature. The mixture was then stirred at room temperature for 17 hours. The reaction was quenched by careful, successive, dropwise addition of water (0.2 mL), 15% NaOH aqueous solution (0.2 mL), and water (0.6 mL). The solid was filtered and washed with MeOH and CH2Cl2. The filtrate was concentrated to dryness, and dried under vacuum, to give 5-bromo-2-pyrrolidin-1-ylmethyl-1H-indole as a white solid. Yield: 0.45 g (90%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09238640B2 |
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| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-86cf673281594b42bc32b56e1de6efda |
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| 出典メモ | uspto-grants-2016_01 |
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