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Hydrogen Bromide → Methyl 3-bromothiophene-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Bromide | HCID 260 | — |
| 反応物 | Methyl 3-amino-2-thiophenecarboxylate | HCID 89652 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 触媒 | copper(I) bromide | HCID 24593 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Methyl 3-bromothiophene-2-carboxylate | HCID 2740074 | — |
反応手順
3-Amino-2-thiophenecarboxylic acid methyl ester (9.4 g) was suspended in hydrobromic acid (20 ml), and the mixture was stirred at room temperature for 30 minutes. The mixture was cooled to 0° C., and sodium nitrite (4.2 g) in water (10 ml) was added dropwise below 10° C. The mixture was stirred for 1 hour, and then poured into copper (I) bromide (9.06 g) in hydrobromic acid (25 ml). The resulting mixture was stirred at 60° C. for 1 hour and extracted with diethyl ether. The extract was dried over anhydrous magnesium sulfate and concentrated under reduced pressure and distilled under reduced pressure to give 3-bromo-2-thiophenecarboxylic acid methyl ester (7.99 g) as crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05840917 |
| 出典データセット | uspto-grants-1998_11 |
| ORD ID | ord-ec300f324c5e47d9a60218fa5b962921 |
| 出典メモ | uspto-grants-1998_11 |