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Water → 1-Bromo-2-methoxy-3-nitrobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Bromo-6-nitrophenol | HCID 13545453 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Bromo-2-methoxy-3-nitrobenzene | HCID 22505713 | — |
反応手順
2-Bromo-6-nitrophenol (5.1 g, 23.4 mmol) was dissolved in DMF (60 mL), then 95% NaH (900 mg, 35.6 mmol) was added in a few portions, followed by the addition of iodomethane (3.0 mL, 6.8 g, 48.5 mmol). The reaction was stirred at room temperature overnight, then heated at 50° C. for 3 hours. The reaction was cooled, poured into water, and the solids filtered off and dried. The product (5.5 g, 100%) was recovered as tan solids. 1H NMR (300 MHz, DMSO-d6) δ 8.02 (dd, J=8.1, 1.7 Hz, 1H), 7.96 (dd, J=8.1, 1.7 Hz, 1H), 7.83 (dd, 8.1, 8.1 Hz, 1H), 3.92 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07456169B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-d03ed043ac1a41c886c1001eaa0187a2 |
| 出典メモ | uspto-grants-2008_11 |