関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2,6-Difluorobenzaldehyde | HCID 136284 | — |
| 反応物 | 4-Methanesulfonylpiperidine hydrochloride | HCID 23061698 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Fluoro-6-(4-methanesulfonylpiperidine-1-yl)benzaldehyde | HCID 58137962 | 84% |
反応手順
In a 250 mL round bottom flask, 2,6-difluorobenzaldehyde (7.12 g, 5.4 mL, 50.1 mmol), 4-methanesulfonylpiperidine hydrochloride (10 g, 50.1 mmol) and DIPEA (7.77 g, 60.1 mmol) were combined with acetonitrile (75 mL). The mixture was stirred and heated at 80° C. overnight. The mixture was evaporated and extracted with dichloromethane and citric acid solution. The organic layer was washed with brine, dried over sodium sulfate, and evaporated. The crude solid was triturated with cold ethyl acetate to afford 2-fluoro-6-(4-methanesulfonylpiperidine-1-yl)benzaldehyde (12 g, 84% yield). LC-MS calcd for C13H16FNO3S (m/e) 285.08, obsd 286.0 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08536172B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-7604022984de470db2eaaeb7e6b15206 |
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| 出典メモ | uspto-grants-2013_09 |
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