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Methyl iodide → 1-Bromo-2-methoxy-5-methyl-3-nitrobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Bromo-4-methyl-6-nitrophenol | HCID 29918 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 1-Bromo-2-methoxy-5-methyl-3-nitrobenzene | HCID 13860183 | 97.9% |
反応手順
2-Bromo-4-methyl-6-nitro-phenol 11b (22.24 g, 95.9 mmol) was dissolved in 150 mL of acetone, followed by addition of potassium carbonate (15.9 g, 115 mmol) and iodomethane (13.7 mL, 220.6 mmol). The reaction mixture was heated to reflux overnight. The reaction was monitored by TLC until the disappearance of the starting materials. The mixture was filtered and the filtrate was concentrated under reduced pressure. The residue was diluted with 100 mL of ethyl acetate and filtered. The mixture was concentrated under reduced pressure to obtain the title compound 1-bromo-2-methoxy-5-methyl-3-nitro-benzene 11c (23.1 g, yield 97.9%) as an orange solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08367710B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-143aadf36a0342eeb5c2baaea9543ba4 |
| 出典メモ | uspto-grants-2013_02 |