関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexamethylphosphoramide | HCID 12679 | — |
| 反応物 | 1-Bromoadamantane | HCID 79106 | — |
| 反応物 | 3-Bromo-2-methylphenol | HCID 11171430 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | HCID 86681263 | HCID 86681263 | — |
反応手順
3-Bromo-2-methylphenol (1000 mg) and 1-bromoadamantane (2013 mg) were added to hexamethylphosphoramide (8 mL) and the mixture was heated in a microwave reactor (Biotage) at 250° C. for 35 minutes. The solution was taken up in diethyl ether, washed with water two times, washed with brine, dried on anhydrous sodium sulfate, filtered, and concentrated. The crude material was purified by flash column chromatography on silica gel using 2% ethyl acetate (hexanes) increasing to 5% ethyl acetate (hexanes) to yield the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08889675B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-32df780e4a2c43c38b62dc29c3a6c1f6 |
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| 出典メモ | uspto-grants-2014_11 |
|---|