참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 3,5-Dimethyl-4-nitrophenol | HCID 138466 | — |
| 반응물 | 5-chloro-N-methyl-2-nitroaniline | HCID 258041 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 용매 | Dimethylacetamide | HCID 31374 | — |
| 생성물 | N-[5-(3,5-Dimethyl-4-nitrophenoxy)-2-nitrophenyl]-N-methylamine | HCID 86233418 | 80.4% |
반응 단계
To a solution of N-(5-chloro-2-nitrophenyl)-N-methylamine (0.86 g) and 3,5-dimethyl-4-nitrophenol (0.76 g) in N,N-dimethylacetamide (12 ml) was added potassium t-butoxide (0.554 g) at room temperature, and the resulting mixture was stirred successively at the same temperature for 20 minutes, at 100° C. for 10 minutes, at 125° C. for 45 minutes, and at 140° C. for 1 hour. After cooling the reaction mixture to 0° C., the reaction mixture was adjusted to a pH of about 3 with 3N hydrochloric acid. The crystalline solid precipitated was collected by filtration, washed successively with 3N hydrochloric acid and water and air-dried for 3 days to afford the title compound (1.16 g, yield: 80%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07816552B2 |
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| 출처 데이터셋 | uspto-grants-2010_10 |
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| ORD ID | ord-281f901f884b469781cb709e98f6a940 |
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| 출처 메모 | uspto-grants-2010_10 |
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