Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Nitrogen → N-(3',4'-difluoro-5-nitrobiphenyl-3-yl)acetamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Nitrogen | HCID 947 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 3,4-Difluorobenzeneboronic acid | HCID 2734337 | — |
| 반응물 | N-(3-bromo-5-nitrophenyl)acetamide | HCID 10658908 | — |
| 촉매 | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| 용매 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 생성물 | N-(3',4'-difluoro-5-nitrobiphenyl-3-yl)acetamide | HCID 117777845 | 76% |
반응 단계
A solution of N-(3-bromo-5-nitrophenyl)acetamide of Example 1(c) (0.7 g, 2.69 mmol) in 1,2-dimethoxyethane (15 ml) was degassed by N2 bubbling for 5 min. 3,4-Difluorophenylboronic acid (0.5 g, 3.23 mmol, 1.2 eq.) was added and the mixture was degassed for another 5 min. Pd(dppf)Cl2 (0.44 g, 0.54 mmol, 0.2 eq.) and aqueous sodium carbonate (0.86 g, 8.07 mmol, 3.0 eq.) were added and the procedure of Example 1(d) was followed. The crude residue of the product was purified by column chromatography (60-120 silica gel, 25% ethyl acetate in hexane) to give the product in 76% yield (0.6 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09447091B2 |
| 출처 데이터셋 | uspto-grants-2016_09 |
| ORD ID | ord-06b0436da7f34efaaf0a773e31cd3b07 |
| 출처 메모 | uspto-grants-2016_09 |