関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | 2,4-Dichloronitrobenzene | HCID 11899 | — |
| 反応物 | 4-Amino-3,5-dimethylphenol | HCID 76543 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | 2,6-Dimethyl-4-[3-(methylamino)-4-nitrophenoxy]aniline | HCID 66701665 | 67% |
反応手順
To a solution of 2,4-dichloronitrobenzene (3.0 g) in N,N-dimethylacetamide (30 ml) was added a 40% aqueous solution of methylamine (4.9 g) at room temperature, and the resulting mixture was stirred at 75-80° C. for 1.5 hours. To the reaction mixture were added 4-amino-3,5-dimethylphenol (2.2 g), potassium t-butoxide (3.5 g), and N,N-dimethylacetamide (15 ml), and the resulting mixture was stirred at the same temperature for 3 hours. After stirring, water (60 ml) was added to the reaction mixture, and the resulting mixture was cooled gradually to room temperature. The crystalline solid precipitated was collected by filtration and dried in vacuo to afford the title compound (3.0 g, yield: 67%) as a yellow crystalline solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08106079B2 |
|---|
| 出典データセット | uspto-grants-2012_01 |
|---|
| ORD ID | ord-60ec85ea250846e98d6e30b990b75e47 |
|---|
| 出典メモ | uspto-grants-2012_01 |
|---|