関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus tribromide | HCID 24614 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Methyl 5-(hydroxymethyl)thiophene-2-carboxylate | HCID 23158735 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 5-(bromomethyl)thiophene-2-carboxylate | HCID 11424851 | — |
反応手順
To an ice-cold solution of methyl 5-(hydroxymethyl)thiophene-2-carboxylate (375 mg, 2.17 mmol) in methylene chloride (9.0 mL) is added phosphorus tribromide (100 μL, 1.08 mmol) and the reaction mixture is stirred at 0° C. for 0.5 h. Saturated sodium bicarbonate (10 mL) is carefully added to the reaction mixture and the phases are separated. The organic phase is washed with water, dried (sodium sulfate), filtered, and concentrated under reduced pressure to yield the title compound in pure form. ESI MS m/z 235 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07727997B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-a9579004e9f04cb59d99e1905f5daad8 |
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| 出典メモ | uspto-grants-2010_06 |
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