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 | 4-Chloro-5-methyl-2-nitrophenol | HCID 23532 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Chloro-4-methoxy-2-methyl-5-nitrobenzene | HCID 15864566 | 87% |
反応手順
To a suspension of sodium hydride (1.2 mmol) in DMF (6 mL), 4-chloro 3-methyl 6-nitrophenol (1.0 mmol) was added at 0° C. The reaction mixture was stirred at 0° C. for 15 minute then methyliodide was added at 0° C. and the mixture was stirred for 4 hours at room temperature. Water (60 mL) was added and the mixture extracted with EtOAc (3×50 mL). The combined organic extracts were washed with water (50 mL), brine (50 mL), dried (Na2SO4) and concentrated under reduced pressure. The residue was purified by column chromatography on silica using 5-8% EtOAc in hexane to give the title compound (87%) as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08716287B2 |
|---|
| 出典データセット | uspto-grants-2014_05 |
|---|
| ORD ID | ord-b4f56fc062134a22a5749301d7d96acf |
|---|
| 出典メモ | uspto-grants-2014_05 |
|---|
