関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Methyl 4-hydroxytetrahydro-2H-thiopyran-3-carboxylate | HCID 10012449 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 4-((methylsulfonyl)oxy)tetrahydro-2H-thiopyran-3-carboxylate | HCID 10377614 | — |
反応手順
A solution of methyl 4-hydroxytetrahydro-2H-thiopyran-3-carboxylate (3.00 g, 17.0 mmol) in DCM (170 mL) was stirred at 0° C. DIPEA (5.95 mL, 34.0 mmol) was added followed by the dropwise addition of methanesulfonyl chloride (1.95 g, 17.0 mmol). The resulting mixture was stirred at 0° C. for 30 minutes then warmed to ambient temperature and stirred for an additional 30 minutes. The mixture was carefully diluted with water and extracted with DCM (2×). The combined organic extracts were washed with 1N aqueous HCl, brine, dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to afford the title compound. The residue was carried forward without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09394282B2 |
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| 出典データセット | uspto-grants-2016_07 |
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| ORD ID | ord-1626c36fd0ff46adad9d07f3cd360440 |
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| 出典メモ | uspto-grants-2016_07 |
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