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Bromine → 3-Bromo-2-hydroxy-5-methoxybenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Sodium Thiosulfate | HCID 24477 | — |
| 反応物 | 2-Hydroxy-5-methoxybenzaldehyde | HCID 95695 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 3-Bromo-2-hydroxy-5-methoxybenzaldehyde | HCID 735818 | 60% |
反応手順
To 2-hydroxy-5-methoxybenzaldehyde (4.1 mL, 32.86 mmol) in acetic acid (150 mL) were added sodium acetate (4.0 g, 49.3 mmol) and bromine (2.2 mL, 42.7 mmol) and the mixture was stirred at rt for 2 h. Aqueous sodium thiosulfate was added and the mixture was concentrated by rotary evaporation. The solid was dissolved in dichloromethane and washed with water. The organic phase was separated, dried over MgSO4, filtered and the solvent removed by rotary evaporation. The solid residue was recrystallized from ethanol to yield 3-bromo-2-hydroxy-5-methoxybenzaldehyde (4.55 g, 60%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08367676B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-61c8486805504bb5aeec8be56df7704d |
| 出典メモ | uspto-grants-2013_02 |