Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Bromo-4-fluoro-2-nitrobenzene → 3-(4-Fluoro-2-nitrophenylamino)-8-nitro-6H-dibenzo[b,e]oxepin-11-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Bromo-4-fluoro-2-nitrobenzene | HCID 2773383 | — |
| 반응물 | 2-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl | HCID 11155794 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 반응물 | 3-Amino-8-nitro-6H-dibenzo[b,e]oxepin-11-one | HCID 67361719 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | tert-Butanol | HCID 6386 | — |
| 생성물 | 3-(4-Fluoro-2-nitrophenylamino)-8-nitro-6H-dibenzo[b,e]oxepin-11-one | HCID 86664810 | — |
반응 조건
| 온도 | 100 °C |
|---|
반응 단계
In accordance with general method Z, 0.85 g (3.14 mmol) of (6), 0.70 g (3.19 mmol) of 1-bromo-4-fluoro-2-nitrobenzene, 2 spatula tips of Pd(OAc)2, 0.10 g of 2-(dicyclohexylphosphino)-2′,4′,6′-triisopropylbiphenyl (phosphine ligand), 0.70 g of KOt-Bu, 2.0 ml of t-BuOH are weighed out and dissolved in 10 ml of toluene (anhydrous). The mixture is refluxed at 100° C. under an argon atmosphere for 4 h. The crude product is purified by chromatography over silica gel with MC/EtOH (98/2). Yield: 0.10 g (7.8%); melting point 210.7° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08633312B2 |
| 출처 데이터셋 | uspto-grants-2014_01 |
| ORD ID | ord-b0aeb9943499427782f937dd0d39c6e5 |
| 출처 메모 | uspto-grants-2014_01 |