関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 2-Fluorobenzenesulphonyl chloride | HCID 137761 | — |
| 反応物 | (3-Amino-2-fluoro-phenyl)-(5-bromo-1H-pyrrolo[2,3-b]pyridin-3-yl)-methanone | HCID 58368906 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 58368734 | HCID 58368734 | 71.5% |
反応手順
To (3-amino-2-fluoro-phenyl)-(5-bromo-1H-pyrrolo[2,3-b]pyridin-3-yl)-methanone (19, 53 mg, 0.159 mmol) in 0.63 mL of tetrahydrofuran, pyridine (0.115 mL, 1.43 mmol) is added, followed by 2-fluorobenzenesulfonyl chloride (20, 46 mg, 0.238 mmol) and the reaction is stirred at room temperature for 48 hours. Hydrochloric acid (1M aqueous) is added to adjust the mixture to pH 4, and the mixture is extracted with ethyl acetate. The organic layer is washed with brine, dried over sodium sulfate, filtered and the filtrate is concentrated under vacuum. The resulting material is purified by silica gel column chromatography, eluting with ethyl acetate and dichloromethane. Appropriate fractions are combined and concentrated under vacuum to provide the desired compound (21, 56 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09440969B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-ba7ceb1933c64dd387f17d429781fba7 |
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| 出典メモ | uspto-grants-2016_09 |
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