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5-Bromo-2-furanecarboxylic acid → Methyl 5-bromofuran-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 5-Bromo-2-furanecarboxylic acid | HCID 68511 | — |
| 反応物 | Boron, trifluoro(methanol)-, (T-4)- | HCID 11062313 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl 5-bromofuran-2-carboxylate | HCID 599633 | — |
反応手順
Boron trifluoride methanol (6.3 ml, 7.6 g) was added to a stirred solution of 5-bromofuran-2-carboxylic acid (10 g) in methanol (90 ml) and heated under reflux under nitrogen for 5 hours. More boron trifluoride methanol (5 ml) was added and the mixture heated under reflux for 5 hours, allowed to cool to room temperature and stand for 10 hours before the solvent was removed in vacuo and the residue poured into saturated sodium hydrogen carbonate solution (300 ml) and extracted with ethyl acetate (3×200 ml). The extract was washed with saturated sodium hydrogen carbonate solution (2×100 ml), dried over MgSO4, and the solvent removed in vacuo to give methyl 5-bromofuran-2-carboxylate, m.p. 62° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04983619 |
| 出典データセット | uspto-grants-1991_01 |
| ORD ID | ord-347464d7359a4fd8b895aa8d88b094e5 |
| 出典メモ | uspto-grants-1991_01 |