Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2,4-Difluoronitrobenzene → 2-(5-Fluoro-2-nitro-phenylamino)-thiophene-3-carbonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2,4-Difluoronitrobenzene | HCID 67967 | — |
| 반응물 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 반응물 | 2-Aminothiophene-3-carbonitrile | HCID 736607 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 2-(5-Fluoro-2-nitro-phenylamino)-thiophene-3-carbonitrile | HCID 69211850 | 45% |
반응 단계
Combine 2,4-difluoro-1-nitro-benzene (5.24 g, 32.94 mmol), 2-aminothiophene-3-carbonitrile (4.09 g, 32.94 mmol), and DMSO (30.0 ml). Add lithium hydroxide monohydrate (2.76 g, 65.88 mmol) all at once and then stir the mixture at 55° for 22 hours. Cool the mixture to ambient temperature and then pour it onto ice chips. Extract with ethyl acetate and then wash (brine), dry (sodium sulfate), and evaporate the organic to residue. Purify the residue on silica gel using hexanes/dichloromethane (35:65) to give 3.89 g (45%) of the title compound as a red solid: mass spectrum (ion spray): m/z=262.0 (M−1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07384934B2 |
| 출처 데이터셋 | uspto-grants-2008_06 |
| ORD ID | ord-2c4b8a4f82994450bcaa96a83066b968 |
| 출처 메모 | uspto-grants-2008_06 |