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Dichloromethane → 5-Bromo-2,3-dimethoxypyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 2,3-Dimethoxypyridine | HCID 4657809 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | 5-Bromo-2,3-dimethoxypyridine | HCID 12563084 | 64.9% |
反応手順
To a 100 mL round-bottomed flask was added 2,3-dimethoxypyridine (2 mL, 15 mmol, Alfa Aesar, Ward Hill, Mass.), CH2Cl2 (30 mL), and bromine (0.7 mL, 14 mmol). The reaction mixture was stirred at rt for 16 h. The reaction mixture was then diluted with sat. NaHCO3 (30 mL) and extracted with EtOAc (2×50 mL). The combined organic extracts were washed with sat. NaCl (20 mL), dried over Na2SO4, filtered and concentrated. Purification by silica gel chromatography (50% CH2Cl2/hexanes) afforded the title compound (1.98 g, 60%). MS (ESI, positive ion) m/z: 218 (M(79Br)+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07820665B2 |
| 出典データセット | uspto-grants-2010_10 |
| ORD ID | ord-08016a45d69e42e1b8eee1f95839037d |
| 出典メモ | uspto-grants-2010_10 |