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Water → 3-Fluoropropyl methanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | 3-Fluoro-1-propanol | HCID 68042 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Fluoropropyl methanesulfonate | HCID 248388 | 91.6% |
反応手順
A solution of 3-fluoro-propan-1-ol (31.2 g, 400 mmol) in 300 mL of CH2Cl2 was treated with methanesulfonyl chloride (55 g, 38 mL, 480 mmol, 1.2 equiv) at 0° C. The resulting reaction mixture was gradually warmed to room temperature and stirred for 1-2 hours. When 1H NMR showed the reaction was complete, the reaction mixture was treated with H2O (100 mL), and the two layers were separated. The aqueous layer was extracted with CH2Cl2 (2×100 mL). The combined organic layers were washed with H2O (3×100 mL) and dried over MgSO4. The solvent was removed in vacuo to afford the desired methanesulfonic acid 3-fluoro-propyl ester (57.2 g, 91% yield) as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08895741B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-7950e57dd2d04a54956cc3e31cfa68c5 |
| 出典メモ | uspto-grants-2014_11 |