関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 6,7-dihydro-4H-thieno[3,2-c]pyran | HCID 11469118 | — |
| 反応物 | Triphenylphosphane dibromide | HCID 12890784 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-(2-Bromoethyl)-3-(bromomethyl)thiophene | HCID 69311722 | 81.5% |
反応手順
To a solution of 9.5 g of triphenylphosphine dibromide dissolved in 50 mL of acetonitrile, 2 g of 6,7-dihydro-4H-thieno[3,2-c]pyrane obtained in Example 14 was added, and the resulting mixture was refluxed for 8 hours. The reaction product solution was concentrated by evaporation under reduced pressure. To the residue, 5 mL of ethyl acetate and then 15 mL of n-hexane were added. The resulting mixture was stirred for 1 hour at room temperature and 2 hours at below 5° C., filtered, and concentrated under reduced pressure. The residue was subjected to a silica gel column chromatography (eluent, n-hexane:ethyl acetate=10:1) to obtain 3.3 g (yield of 80%) of the title compound as a yellowish oil, of which analysis data were the same as obtained in Example 7.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07449580B2 |
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| 出典データセット | uspto-grants-2008_11 |
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| ORD ID | ord-0290745d991240f6b8b001632ca5e50e |
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| 出典メモ | uspto-grants-2008_11 |
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