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Formaldehyde → 2-Hydroxy-4-iodobenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Iodophenol | HCID 12272 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Magnesium Chloride | HCID 5360315 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Hydroxy-4-iodobenzaldehyde | HCID 18351513 | 160.1% |
反応手順
To a solution of 3-iodophenol (3.00 g, 13.6 mmol) in acetonitrile (50 mL) was added magnesium chloride (3.89 g, 40.9 mmol), triethylamine (7.6 mL, 55 mmol), and paraformaldehyde (1.64 g, 55 mmol). The reaction mixture was refluxed overnight, then neutralized with saturated aqueous ammonium chloride. The resultant red precipitate was removed by filtration, and the filtrate was extracted with ethyl acetate. The precipitate was dissolved in methanol and added to the combined organic extracts, which were then dried over magnesium sulfate. The solvent was removed under reduced pressure to provide an orange solid (5.4 g) as the crude product. This material was used in the subsequent step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07420066B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-02721cc0f01345be9e12390ff0c5239e |
| 出典メモ | uspto-grants-2008_09 |