関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Solketal | HCID 7528 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (2,2-Dimethyl-1,3-dioxolan-4-yl)methyl methanesulfonate | HCID 15570840 | — |
反応手順
To a solution of (2,2-dimethyl-[1,3]dioxolan-4-yl)-methanol (1.25 g, 9.46 mmol) and triethylamine (9.2 ml, 66.2 mmol) in dichloromethane (60 ml) at 0° C. was slowly added methanesulfonyl chloride (2.2 ml, 28.4 mmol). The reaction mixture was stirred at 0° C. for 2 h then quenched with water and the aqueous layer was extracted with dichloromethane. The combined organics were washed with 10% citric acid, sat NaHCO3, and brine then dried over MgSO4 and concentrated to afford methanesulfonic acid 2,2-dimethyl-[1,3]dioxolan-4-ylmethyl ester as a light brown oil which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08658646B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-402d486a81b84fbaa9544902b15926cb |
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| 出典メモ | uspto-grants-2014_02 |
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