化工社化工社 化学情報印刷レポート · 研究参考用
Methanol → 6-Chloro-2-methoxy-3-nitropyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2,6-Dichloro-3-nitropyridine | HCID 85239 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | 6-Chloro-2-methoxy-3-nitropyridine | HCID 10797703 | — |
反応手順
To a suspension of sodium hydride (684 mg, 28.49 mmol) in xylene (100 ml), methanol (0.98 ml, 25.9 mmol) in xylene (30 ml) was added under nitrogen. The mixture was stirred for 20 min. A solution of 2,6-dichloro-3-nitropyridine (5.0 g, 25.9 mmo) in xylene (100 ml) was added to the reaction mixture and stirred at room temperature overnight. Water (50 ml) was added and the organic layer was separated. The organics was washed with water (1×50 ml) and brine (2×50 ml), dried, and concentrated in vacuo. The crude product was purified by flash chromatography (10:1 methylene chloride and acetone) to provide the desired compound, 6-chloro-2-methoxy-3-nitro-pyridine, as the only isomer as light yellow solid (90%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07425557B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-f960d4a592e84bd0a048645b99309520 |
| 出典メモ | uspto-grants-2008_09 |