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Pyridine → 1-[2-(5-Bromo-pyridin-3-yl)-pyrrolidin-1-yl]-ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 3-Bromo-5-(pyrrolidin-2-yl)pyridine | HCID 4403815 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-[2-(5-Bromo-pyridin-3-yl)-pyrrolidin-1-yl]-ethanone | HCID 117667240 | 132% |
反応手順
To a solution of 3-bromo-5-(2-pyrrolidinyl)pyridine (200 mg, 0.881 mmol) and pyridine (0.2 mL, 1.96 mmol) in DCM (1 mL) in a 8-mL vial is added acetic anhydride (0.093 mL, 0.969 mmol) dropwise. The mixture is stirred at room temperature for 2.5 h. The mixture is concentrated. The resulting crude product is purified by normal phase chromatography using 0-4.5% MeOH in DCM as the gradient to afford 1-[2-(5-bromo-pyridin-3-yl)-pyrrolidin-1-yl]-ethanone (313 mg, 83% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09181272B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-621fe542518d4dd4a7d446037a497fb3 |
| 出典メモ | uspto-grants-2015_11 |