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Ethyl Acetate → 1-(4-Methoxybenzyl)-5-bromo-4-methyl-3-nitro-2-pyridone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Methyloxybenzyl chloride | HCID 69993 | — |
| 反応物 | 5-Bromo-2-hydroxy-4-methyl-3-nitropyridine | HCID 21706517 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(4-Methoxybenzyl)-5-bromo-4-methyl-3-nitro-2-pyridone | HCID 21706479 | 68% |
反応手順
To a stirred solution of 5-bromo-4-methyl-3-nitro-2-pyridone (0.60 g, 2.5 mmol) in DMF (15 mL) was added sodium hydride (60% suspension in oil, 0.103 g). After 30 minutes, 4-methoxybenzyl chloride (0.35 mL) was added, and the mixture was stirred overnight at rt. Ethyl acetate was added and the organic phase was washed with water, dried (Na2SO4), filtered and evaporated. Chromatography of the residue over silica gel (ethyl acetate/hexane 1/1)) gave 1-(4-methoxybenzyl)-5-bromo-4-methyl-3-nitro-2-pyridone (0.60 g, 1.7 mmol, 68%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06268365B1 |
| 出典データセット | uspto-grants-2001_07 |
| ORD ID | ord-a2fc566f34854035be24dc6d451663a6 |
| 出典メモ | uspto-grants-2001_07 |