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Water → 6-Nitro-o-anisidine
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 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Amino-3-Nitrophenol | HCID 4115495 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-Nitro-o-anisidine | HCID 85491 | 90.5% |
反応手順
To a mixture of 2-amino-3-nitrophenol (19.25 g) and K2CO3 (19 g) in DMF (100 mL) was added MeI (11 mL) at room temperature and the mixture was stirred over night and then poured into water. The resulting precipitate was collected by filtration and the solid was washed with water to afford the desired product (19 g, 90%). 1H NMR (300 MHz, CDCl3) δ ppm 3.92 (s, 1H), 6.43 (br s, 1H), 6.61 (dd, 1H, J=7.5, 9.0 Hz), 6.89 (dd, 1H, J=0.9, 7.5 Hz), 7.73 (dd, 1H, J=0.9, 9.0 Hz); LC-MS: m/e=169 [M+1]+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541411B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-5902f394338943068ba0956c4d2c0bee |
| 出典メモ | uspto-grants-2013_09 |