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Acetyl chloride → 4-Chloro-2-methyl-1-oxo-1lambda~5~-pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Pyridine, 2-methyl-4-nitro-, 1-oxide | HCID 95291 | — |
| 生成物 | 4-Chloro-2-methyl-1-oxo-1lambda~5~-pyridine | HCID 12211801 | 32.7% |
反応手順
15.4 g (0.1 mol) of 2-methyl-4-nitropyridine 1-oxide was added to 78.5 g (1 mol) of acetyl chloride at -10° C. The obtained mixture was stirred under cooling with ice for 0.5 hour. After the completion of the reaction, 300 ml of ice-water was added to the reaction mixture. The obtained mixture was neutralized with sodium carbonate and extracted with chloroform. The extract was dried over magnesium sulfate and filtered. The filtrate was concentrated under a reduced pressure and purified by silica gel column chromatography (ethyl acetate/n-hexane/methanol) to obtain 4.7 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05840910 |
| 出典データセット | uspto-grants-1998_11 |
| ORD ID | ord-743aec568dbb4f9fb0d7ff56d8c684aa |
| 出典メモ | uspto-grants-1998_11 |