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Sodium Carbonate → 5-Bromo-2-fluoro-3-pyridinecarboxaldehyde oxime
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | 5-Bromo-2-fluoro-3-pyridinecarboxaldehyde | HCID 45480192 | — |
| 溶媒 | Methanol--water (1/1) | HCID 22242641 | — |
| 生成物 | 5-Bromo-2-fluoro-3-pyridinecarboxaldehyde oxime | HCID 131736879 | 97.8% |
反応手順
To a solution of 5-bromo-2-fluoro-pyridine-3-carbaldehyde (2) (20.0 g, 98.0 mmol) in 1:1 MeOH—H2O (250 mL) was added hydroxylamine hydrochloride (7.52 g, 108 mmol) and sodium carbonate (11.4 g, 108 mmol). The reaction mixture was stirred at rt for 1 hour. The solvent was evaporated in vacuo and the residue diluted with H2O (200 mL) and EtOAc (200 mL). The organic phase was separated, dried (Na2SO4), filtered and the solvent evaporated in vacuo. The product was obtained as a light pink solid (21.0 g, 93%); Rf: 0.4 (10% EtOAc-pet ether).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09433622B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-e1b82a2e6c5043789b778fa207d56113 |
| 出典メモ | uspto-grants-2016_09 |