関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4,4'-Dibromo-2,2'-bis-hydroxymethyl-biphenyl | HCID 11372175 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Phosphoric Acid | HCID 1004 | — |
| 生成物 | 3,9-Dibromo-5,7-dihydrodibenzo[c,e]oxepine | HCID 22316165 | 95% |
反応手順
The suspension of (4,4′-dibromo-2′-hydroxymethyl-biphenyl-2-yl)-methanol (460 mg) in phosphoric acid (25 ml) was heated at 160° C. for 4 hours. The mixture was cooled and diluted with water (100 ml), and was extracted with EtOAC. The organic phase was washed with water, saturated sodium bicarbonate, and brine, and was dried with sodium sulfate. Concentration yielded 3,9-dibromo-5,7-dihydro-dibenzo[c,e]oxepine (416 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822430B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-491a4729ede64f0386a987b8ac9d7963 |
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| 出典メモ | uspto-grants-2014_09 |
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