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Triethylamine → 1-(Methylsulfonyl)piperidin-4-yl methanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | Piperidin-4-ol | HCID 79341 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(Methylsulfonyl)piperidin-4-yl methanesulfonate | HCID 22273065 | 89% |
反応手順
To a solution of 4-hydroxypiperidine (5.10 g, 50 mmoles) and triethylamine (20.9 ml, 150 mmoles) in methylene chloride (150 ml) was added methanesulfonyl chloride (8.54 ml, 110 mmoles) with stirring under ice-cooling and the mixture was stirred at room temperature for 1 hour. The reaction mixture was washed in turn with an aqueous saturated sodium bicarbonate solution and saturated saline and dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was solidified with ethyl acetate-n-hexane to obtain 11.45 g of the desired product (88.3%, pale yellow solid).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05244908 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-000317cc53274835920257e50a875bf5 |
| 出典メモ | uspto-grants-1993_09 |