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-[2-(Cyclopropylmethoxy)phenoxy]ethan-1-OL | HCID 19919928 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-[2-(Cyclopropylmethyloxy)phenoxy]ethyl methanesulfonate | HCID 15289625 | 99.2% |
反応手順
2-Cyclopropylmethyloxy-1-(2-hydroxyethyloxy)benzene (2.7 g, 13.0 mmol), prepared as in Example 1, Step (a), and triethylamine (2.7 mL, 19.5 mmol) were dissolved in methylene chloride (20 mL) and the solution was cooled in an ice bath. Methanesulfonyl chloride (1.2 mL, 15.5 mmol) in methylene chloride (10 mL) was added dropwise to the solution and the mixture was stirred at 0° C. for 30 minutes. Water was added and the mixture was stirred vigorously at room temperature for 15 minutes. The mixture was extracted into methylene chloride. The organic phase was separated, washed with 2N hydrochloric acid and then brine, and dried over magnesium sulfate. Evaporation gave 2-[2-(cyclopropylmethyloxy)phenoxy]ethyl methanesulfonate (3.7 g, 12.9 mmol) as a white solid, m.p. 90°-91° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05436264 |
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| 出典データセット | uspto-grants-1995_07 |
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| ORD ID | ord-41b83493471243339b47beefd2585755 |
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| 出典メモ | uspto-grants-1995_07 |
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