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HRID 337587作成日:2026年10月26日
Dichloromethane → 2-[3,4-Dichloro-5-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)phenyl]ethyl methanesulfonate
https://huagongshe.com/reaction/337587
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-[3,4-Dichloro-5-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)phenyl]ethanol | HCID 66895403 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-[3,4-Dichloro-5-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)phenyl]ethyl methanesulfonate | HCID 86651668 | — |
反応手順
To a dichloromethane (0.11 M) solution of 2-[3,4-dichloro-5-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)phenyl]ethanol (1 eq.) from the previous step was added at 0° C. Hunig's base (1.5 eq.) and methanesulfonyl chloride (1.1 eq.). The resulting suspension was stirred at 0° C. for 30 min and at RT for 15 min. The reaction was then diluted with ether and quenched with 1N aq. HCl. The aqueous layer was separated and back-extracted with ether. The combined organic extracts were washed further with 1 N aq. NaOH, water and brine, dried over Na2SO4, filtered and the filtrate concentrated in vacuo to give the title compound as a brown oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08889714B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-ba30d19d5c82457cabbcda5757a1e3a4 |
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| 出典メモ | uspto-grants-2014_11 |
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