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Water → 2-Cyclopropylethyl methanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | 2-Cyclopropylethan-1-ol | HCID 137642 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Cyclopropylethyl methanesulfonate | HCID 14557809 | 99.8% |
反応手順
To a solution of 2-cyclopropylethanol (2.1 g, 24.4 mmol) in dichloromethane (50 ml) at 0° C. under nitrogen was added triethylamine (4.1 ml, 1.2 mol. equiv.). Methanesulphonyl chloride (2.5 ml, 1.3 mol. equiv.) was added, dropwise, and the reaction allowed to stir for 18 hours at room temperature. Water (50 ml) and dichloromethane (50 ml) were added. The organic phase was separated, washed with water (2×50 ml) and then dried over anhydrous sodium sulphate. The solution was filtered and the solvent removed from the filtrate by evaporation under reduced pressure to give the title compound as an oil (4 g). TLC Rf=0.9 (silica, methanol:dichloromethane, 1:19, by volume). LRMS m/z=182 (m+18)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06262075B1 |
| 出典データセット | uspto-grants-2001_07 |
| ORD ID | ord-ecfd5f27621649f6ba2ed88a7ea7819e |
| 出典メモ | uspto-grants-2001_07 |