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Methyl iodide → Methyl 4-bromo-3-methoxythiophene-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Methyl 4-bromo-3-hydroxythiophene-2-carboxylate | HCID 2777611 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | Methyl 4-bromo-3-methoxythiophene-2-carboxylate | HCID 2736824 | 129.3% |
反応手順
Methyl-3-hydroxy-4-bromo-2-thiophenecarboxylate (10.0 g, 42.2 mmol) was dissolved in 250 mL of acetone. Potassium carbonate (30.0 g, 217.4 mmol) was added followed by a solution of iodomethane (14.5 mL, 233.0 mmol). The mixture was heated to reflux and continued for 6 h. After cooled to room temperature, the mixture was filtered, the solid material was rinsed with acetone (˜200 mL). The filtrate and rinsing were concentrated under reduced pressure to a solid, further dried on high vacuum, yielding 13.7 g (100%) of methyl-3-methoxy-4-bromo-2-thiophenecarboxylate (MH+=251.0),
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07786149B2 |
| 出典データセット | uspto-grants-2010_08 |
| ORD ID | ord-9f6de7ac8dde43f9b1464dc0799a33c6 |
| 出典メモ | uspto-grants-2010_08 |