関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Tyrosol | HCID 10393 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(Methylsulfonyloxy)-2-[4-(methylsulfonyloxy)phenyl]ethane | HCID 11220122 | — |
反応手順
2-(4-Hydroxyphenyl)ethanol(356 g, 2.58 mol, 1.0 eq) was dissolved in methylene chloride (3500 ml) and triethyl amine (653 g, 6.44 mol, 2.5 eq). The mixture was cooled to −20° C. Methanesulfonyl chloride (657 g, 5.74 mol. 2.2 eq) was then added keeping the temperature between −25° C. and −15° C. When the conversion was >95% salts were formed which were filtered off and washed with methylene chloride (600 ml). The organic layer was washed first with saturated sodium hydrogencarbonate solution (700 ml) at 20° C. followed by water (700 ml). The methylene chloride was evaporated to dryness and the remaining residue was then used in the subsequent step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07084177B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-cdfc09446c49400d80ac411e2e633a6a |
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| 出典メモ | uspto-grants-2006_08 |
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