関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Amino-3,5-dimethylphenol | HCID 76543 | — |
| 反応物 | 5-chloro-N-methyl-2-nitroaniline | HCID 258041 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 触媒 | 2,6-Di-tert-butyl-4-methylphenol | HCID 31404 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | 2,6-Dimethyl-4-[3-(methylamino)-4-nitrophenoxy]aniline | HCID 66701665 | 93% |
反応手順
To a solution of N-(5-chloro-2-nitrophenyl)-N-methylamine (8.00 g) in N,N-dimethylacetamide (112 ml) was added 2,6-di-t-butyl-4-methylphenol (0.24 g). Furthermore, to the resulting mixture were added 4-amino-3,5-dimethylphenol (6.47 g) and potassium t-butoxide (5.29 g) with stirring, and the resulting mixture was stirred at 60° C. for 30 minutes. After stirring, water (4 ml) was added to the reaction mixture, and furthermore water (120 ml) was added dropwise over a 2-hour interval, and then the resulting mixture was cooled gradually to room temperature. The crystalline solid precipitated was collected by filtration, washed with water (80 ml) and dried in vacuo to afford the title compound (11.45 g, yield: 93%) as a yellow crystalline solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08106079B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-97c8e7f50c6245feba5e6993c429544a |
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| 出典メモ | uspto-grants-2012_01 |
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