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Potassium Carbonate → 2-Bromo-4-methyl-3-nitro-pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Phosphorus oxybromide | HCID 24613 | — |
| 反応物 | 2-Hydroxy-4-methyl-3-nitropyridine | HCID 345370 | — |
| 溶媒 | 1,1-Dichloroethane | HCID 6365 | — |
| 生成物 | 2-Bromo-4-methyl-3-nitro-pyridine | HCID 19926089 | 71.8% |
反応手順
The 4-methyl-3-nitropyridin-2(1H)-one (110 g, 0.71 mol) was suspended in dichloroethane (1 L). The solution of phosphorus oxybromide (317 g, 1.1 mol) in dichloroethane (1 L) was added dropwise thereto at the ambient temperature. The reaction mixture was refluxed for 12 hours. The mixture was allowed to cool to room temperature, poured into ice water, and neutralized with potassium carbonate. The organic layer was separated, washed with water and brine, and dried over sodium sulfate. The solvent was evaporated to provide the title compound (yield 71.8%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09440968B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-ebac018909a54f20af991c206b66b15b |
| 出典メモ | uspto-grants-2016_09 |