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 | (R)-1-(6-methylpyridin-2-yl)ethanol | HCID 45079484 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (R)-Methanesulfonic acid 1-(6-methyl-pyridin-2-yl)-ethyl ester | HCID 57656393 | 100% |
反応手順
To a stirred solution of (R)-1-(6-methyl-pyridin-2-yl)-ethanol (175 mg, 1.28 mmol) and triethylamine (355 μl, 2.56 mmol) in DCM (5 mL) at 0° C. add methanesulfonyl chloride (148 μl, 1.92 mmol). Stir at 0° C. for 30 min and quench the reaction mixture with saturated aqueous NaHCO3 at the same temperature. Extract the mixture three times with EtOAc, dry over anhydrous Na2SO4, and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (8:2) to give the title compound as a colorless oil (274 mg, 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08580780B2 |
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| 出典データセット | uspto-grants-2013_11 |
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| ORD ID | ord-3b3589badff448a4b935f28242353b8d |
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| 出典メモ | uspto-grants-2013_11 |
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