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Acetic Anhydride → 1-Acetyl-4-benzoylpiperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 4-Benzoylpiperidine hydrochloride | HCID 2724437 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-Acetyl-4-benzoylpiperidine | HCID 2740714 | — |
反応手順
A mixture of phenyl(piperidin-4-yl)methanone hydrochloride (743 mg, 3.29 mmol, Apollo Scientific) in DCM (13.2 mL) and TEA (1.10 mL, 7.90 mmol) was treated with Ac2O (0.373 mL, 3.95 mmol) dropwise over 1 min on an ice bath under argon, and the resulting translucent mixture was immediately removed from the ice bath and stirred at room temperature overnight. The reaction was then partitioned with 1 M HCl (1×8 mL) and 1 M NaOH (1×8 mL), and the organic layer was dried (Na2SO4), filtered, and concentrated to provide the title compound as a translucent beige oil that crystallized upon standing.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09309222B2 |
| 出典データセット | uspto-grants-2016_04 |
| ORD ID | ord-7e76c6bd2a5040c4997c089712112ea1 |
| 出典メモ | uspto-grants-2016_04 |