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Phosphorus oxychloride → 5-Bromo-2-chloro-3-nitropyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 5-Bromo-3-nitro-2-pyridone | HCID 85147 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-Bromo-2-chloro-3-nitropyridine | HCID 7019412 | 89% |
反応手順
A mixture of 5-bromo-3-nitropyridin-2(1H)-one (Step A, 2.5 g, 10.4 mmol), phosphoryl chloride (25 mL) and N,N-dimethylformamide (2.5 mL) was stirred under reflux for 3 h. After removal of solvent, the residue was dissolved in water (20 mL) and diethylether (20 mL) at 0° C. and the solution was separated. The organic layer was washed with saturated sodium hydrogen carbonate, dried over sodium sulfate and concentrated to afford the title compound (2.5 g, 89%) as a pale yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07598393B2 |
| 出典データセット | uspto-grants-2009_10 |
| ORD ID | ord-676b09dbcdbc4ceeb8a783fc912f8319 |
| 出典メモ | uspto-grants-2009_10 |