関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 3-Fluoro-4-hydroxybenzaldehyde | HCID 587250 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 3-Bromo-5-fluoro-4-hydroxybenzaldehyde | HCID 18701750 | 48% |
反応手順
To a solution of 3-fluoro-4-hydroxybenzaldehyde (2 g, 14.3 mmol, 1 eq, Oakwood Products, Inc., West Columbia, S.C., USA) in acetic acid (60 mL), was added a solution of bromine (2.7 g, 17.0 mmol, 1.2 eq) in acetic acid (10 mL), and the mixture was stirred at 45° C. for 26 h. After concentration in vacuo, brine (50 mL) was added to the residue and the mixture was extracted with EtOAc (3×80 mL). The combined organic layers were dried (Na2SO4), concentrated in vacuo, and purified by reversed phase semi-preparative .HPLC to afford 1.5 g (48%) of 3-bromo-5-fluoro-4-hydroxybenzaldehyde (26).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822467B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-2e1447b6899046a8ae0ab1be7967fba8 |
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| 出典メモ | uspto-grants-2014_09 |
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