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Sodium hydride → 1-(4-Methoxybenzyl)-5-iodo-4-methyl-3-nitro-2-pyridone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Methyloxybenzyl chloride | HCID 69993 | — |
| 反応物 | 5-Iodo-4-methyl-3-nitro-1,2-dihydropyridin-2-one | HCID 21706514 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(4-Methoxybenzyl)-5-iodo-4-methyl-3-nitro-2-pyridone | HCID 21706516 | 75% |
反応手順
A mixture of 5-iodo-4-methyl-3-nitro-2-pyridone (2.90 g, 10.4 mmol) and sodium hydride (60% in oil, 0.44 g, 11 mmol) was stirred at rt for 2.5 hours. 4-Methoxybenzyl chloride (1.50 mL) was added, and the mixture was stirred at rt for 18 h. Water was added, and the mixture and extracted with ethyl acetate. The organic phase was washed, dried and evaporated. Chromatography of the residue over silica gel (35% ethyl acetate/petroleum ether) followed by crystallization from water gave 1-(4-methoxybenzyl)-5-iodo-4-methyl-3-nitro-2-pyridone (3.11 g, 75%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06054470 |
| 出典データセット | uspto-grants-2000_04 |
| ORD ID | ord-909f08c5c24747bd91354eab7a57f8a4 |
| 出典メモ | uspto-grants-2000_04 |