참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 4-Fluoro-2-nitroaniline | HCID 67769 | — |
| 반응물 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 반응물 | 2-Fluoro-5-methylbenzonitrile | HCID 2774584 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-(4-Fluoro-2-nitro-phenylamino)-5-methyl-benzonitrile | HCID 21093460 | 45.2% |
반응 단계
Combine 4-fluoro-2-nitro-phenylamine (2.9 g, 18.50 mmol), 2-fluoro-5-methyl-benzonitrile (2.5 g, 18.50 mmol) and lithium hydroxide monohydrate (2.4 g, 57.20 mmol) in methyl sulfoxide (DMSO, 40 ml). Heat the resulting mixture to 55° C. for 40 hours. Cool the reaction mixture to ambient temperature, then pour into approximately 250 ml of ice water and stir for one hour. Filter the resulting mixture and collect the precipitate. Chromatograph the solid using flash chromatography and elute with mobile phase: 90% hexanes, 5% ethyl acetate, and 5% dichloromethane to obtain 2.267 g of the title compound (8.36 mmol, 45% yield) as an orange amorphous solid: Mass Spectrum (m/e): 272(M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07384934B2 |
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| 출처 데이터셋 | uspto-grants-2008_06 |
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| ORD ID | ord-b3b2628025d8478b9fcf42782ca39456 |
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| 출처 메모 | uspto-grants-2008_06 |
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