関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-((3,4,5-Trimethoxybenzyl)thio)phenol | HCID 384136 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Hydroxy-3,5-dimethoxybenzyl 4-hydroxyphenyl thioether | HCID 15840398 | 63% |
反応手順
3,4,5-Trimethoxybenzyl 4-hydroxyphenyl thioether (3 g, 9.8 mmol), prepared as described in Example 1, was dissolved in 60 ml of dry methylene chloride, and cooled to -78° C. A solution of borontribromide (2.8 ml, 29.5 mmol) in 10 ml of methylene chloride was added dropwise to the above solution. The mixture was stirred to room temperature, and immediately cooled to 0° C. Water (50 ml) was then added dropwise, and the methylene chloride layer was separated. The crude product, obtained after being dried over magnesium sulfate and concentrated, was purified on silica gel column chromatography (ethyl acetate/n-hexane=1/2) to give 1.8 g (63% yield) of 4-hydroxy-3,5-dimethoxybenzyl 4-hydroxyphenyl thioether as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05840991 |
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| 出典データセット | uspto-grants-1998_11 |
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| ORD ID | ord-452f5651b20a4cdf9b9505d7bd5ee1a0 |
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| 出典メモ | uspto-grants-1998_11 |
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