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4-Hydroxybenzaldehyde → 4-Hydroxy-3-iodobenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Hydroxybenzaldehyde | HCID 126 | — |
| 反応物 | N-Iodosuccinimide | HCID 120273 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 4-Hydroxy-3-iodobenzaldehyde | HCID 968881 | 50% |
反応手順
To a stirred solution of 4-hydroxybenzaldehyde (2.0 g, 16.39 mmol) in AcOH (30 mL) was added N-iodosuccinimide (4.5 g, 19.67 mmol). The reaction mixture was stirred at r.t. for 16 h, then filtered. The filtrate was poured onto water (100 mL) and EtOAc (50 mL) was added. The aqueous fraction was separated, then extracted with EtOAc (3×50 mL). The combined organic fractions were washed with water (2×20 mL), dried (Na2SO4), filtered and concentrated in vacuo to give the title compound (2.0 g, 50%) as a white solid that was used without further purification. LCMS (ES−) 247.1 (M−H)−, RT 1.44 minutes (Method 9).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08242116B2 |
| 出典データセット | uspto-grants-2012_08 |
| ORD ID | ord-718e7fa5c9454b87be8d036dbf026bab |
| 出典メモ | uspto-grants-2012_08 |