関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 2-Fluoro-4-hydroxybenzaldehyde | HCID 587246 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 5-Bromo-2-fluoro-4-hydroxybenzaldehyde | HCID 59342578 | 35% |
反応手順
To a solution of 2-fluoro-4-hydroxybenzaldehyde (2.2 g, 15.7 mmol, 1 eq) in acetic acid (70 mL) was added a solution of bromine (2.71 g, 17.0 mmol, 1.1 eq) in acetic acid (10 mL), and the mixture was stirred at 45° C. for 26 h. The reaction was concentrated in vacuo, brine (50 mL) was added, and the mixture was extracted with EtOAc (3×80 mL). The combined organic layers were dried (Na2SO4), concentrated in vacuo. The resultant residue was purified by silica gel chromatography (DCM:MeOH=15:1 to 5:1) to afford 1.2 g (35%) of 5-bromo-2-fluoro-4-hydroxybenzaldehyde (25).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08822467B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-86b166b84f3a4470880b3752f6023d13 |
|---|
| 出典メモ | uspto-grants-2014_09 |
|---|