Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Toluene → 6-methyl-3'-nitro-N-[3-(trifluoromethyl)phenyl]biphenyl-3-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 3-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)nitrobenzene | HCID 11265164 | — |
| 반응물 | 3-iodo-4-methyl-N-(3-(trifluoromethyl)phenyl)benzamide | HCID 17197569 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 6-methyl-3'-nitro-N-[3-(trifluoromethyl)phenyl]biphenyl-3-carboxamide | HCID 69273781 | — |
반응 단계
4,4,5,5-Tetramethyl-2-(3-nitrophenyl)-1,3,2-dioxaborolane (1.4 g, 5.6 mmol) was mixed with 3-iodo-4-methyl-N-[3-(trifluoromethyl)phenyl]benzamide (2.00 g, 4.94 mmol), potassium carbonate (1.4 g, 9.9 mmol), toluene (40 mL), ethanol (6.0 mL), and water (4.0 mL). The mixture was degassed and tetrakis(triphenylphosphine)palladium(0) (0.27 g, 0.24 mmol) was added. The resulting mixture was heated to reflux for 16 hours. The reaction was then cooled and was extracted with ethyl acetate. The organic extracts were washed with water, brine, dried (Na2SO4) and concentrated. The product was purified by flash column chromatography, eluting with a gradient of 20-50% ethyl acetate in hexanes (1.92 g, 91%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08841318B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-4b33ffaa42fa4924988fa781d468829c |
| 출처 메모 | uspto-grants-2014_09 |