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Diethylene Glycol Monomethyl Ether → 2-(2-Methoxyethoxy)ethyl methanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethylene Glycol Monomethyl Ether | HCID 8134 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(2-Methoxyethoxy)ethyl methanesulfonate | HCID 3815654 | — |
反応手順
To a solution of 2-(2-methoxyethoxy)ethanol (300 mg, 2.5 mmol) in DCM (5 mL) was added methanesulfonyl chloride (370 mg, 2.6 mmol) dropwise at 0° C. After stirred at this temperature for 5 min, TEA (505 mg, 5.0 mmol) was added. It was stirred at room temperature overnight. The mixture was partitioned between DCM and water. The organic layers were combined, dried over sodium sulfate, filtered and concentrated to give a crude oil product, which was used without purification. Product tlc [petroleum ether/ethyl acetate [1:1) developed with iodine, Rf 0.5]
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09359359B2 |
| 出典データセット | uspto-grants-2016_06 |
| ORD ID | ord-e134149354544190ab9bd43f7d75f26d |
| 出典メモ | uspto-grants-2016_06 |