化工社化工社 化学情報印刷レポート · 研究参考用
Ethylene Glycol → 1,2-Ethanediol, 1,2-dimethanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 溶媒 | Toluene methylene chloride | HCID 21877217 | — |
| 生成物 | 1,2-Ethanediol, 1,2-dimethanesulfonate | HCID 20796 | — |
反応手順
Potassium carbonate (6.7 g, 48.5 mmol) and diisopropylethylamine (0.3 g, 2.3 mmol) were suspended in dichloromethane-toluene (1/1, 10 mL), and ethylene glycol (1.5 g, 23.3 mmol) and methanesulfonyl chloride (5.5 g, 48.0 mmol) were dropped at the same time in an ice bath. A reaction was effected at room temperature for 3 hours and, thereafter, the reaction was terminated by addition to ice water. An organic layer separated through liquid separation was concentrated, so as to obtain the desired product, 1,2-bis(methanesulfonyloxy)ethane, at a yield of 36% (1.8 g, 8.4 mmol). The measurement result of 1H NMR is as described below.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08716513B2 |
| 出典データセット | uspto-grants-2014_05 |
| ORD ID | ord-d8d69f21d68e4417a51945fb50233f1c |
| 出典メモ | uspto-grants-2014_05 |