참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 4-Amino-3,5-dimethylphenol | HCID 76543 | — |
| 반응물 | 5-chloro-N-methyl-2-nitroaniline | HCID 258041 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 촉매 | 2,6-Di-tert-butyl-4-methylphenol | HCID 31404 | — |
| 용매 | Dimethylacetamide | HCID 31374 | — |
| 생성물 | 2,6-Dimethyl-4-[3-(methylamino)-4-nitrophenoxy]aniline | HCID 66701665 | 93% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08106079B2 |
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| 출처 데이터셋 | uspto-grants-2012_01 |
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| ORD ID | ord-97c8e7f50c6245feba5e6993c429544a |
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| 출처 메모 | uspto-grants-2012_01 |
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