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Dichloromethane → 6-Bromo-5-methoxypicolinaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Potassium Persulfate | HCID 24412 | — |
| 反応物 | 2-Bromo-3-methoxy-6-methylpyridine | HCID 10965563 | — |
| 溶媒 | Acetonitrile--water (1/1) | HCID 18373917 | — |
| 生成物 | 6-Bromo-5-methoxypicolinaldehyde | HCID 22268339 | 24% |
反応手順
A stirred mixture of 2-bromo-3-methoxy-6-methyl-pyridine (2.00 g, 9.9 mmol), Cu(II) sulfate pentahydrate (2.47 g, 9.9 mmol), and potassium peroxydisulfate (8.03 g, 29.7 mmol) in 80 mL of acetonitrile/H2O (1:1) was heated under reflux. After 1 hour, the dark green mixture was cooled to room temperature and CH2Cl2 was added. The layers were separated and the aqueous layer further extracted with CH2Cl2. The organics were combined, dried (MgSO4), filtered and evaporated. The resulting crude product was purified on silica gel [Biotage, hexane:ethyl acetate (4:1)] to give a white solid (0.51 g, 24% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06974826B2 |
| 出典データセット | uspto-grants-2005_12 |
| ORD ID | ord-d064aa9791fb4b8394ad183c1d577c0c |
| 出典メモ | uspto-grants-2005_12 |