Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sulfuric Acid → 6-Bromo-5,7-difluoroquinoline
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Nitrobenzene | HCID 7416 | — |
| 반응물 | 4-Bromo-3,5-difluoroaniline | HCID 2736260 | — |
| 용매 | Glycerol | HCID 753 | — |
| 생성물 | 6-Bromo-5,7-difluoroquinoline | HCID 45108354 | — |
반응 단계
A mixture of 4-bromo-3,5-difluoro-phenylamine (6.0 g, 28.8 mmole), ferrous sulfate (1.82 g), glycerol (8.6 mL), nitrobenzene (1.79 mL) and 5.0 ml of concentrated sulfuric acid (5 mL) was heated gently. After the first vigorous reaction, the mixture was heated to reflux for five hours. Nitrobenzene was removed by distillation in vacuo. The aqueous solution was acidified with glacial acetic acid, and dark brown precipitate separated, which was purified by flash chromatography (silica gel, petroleum/ethyl acetate=12/1) to return the title compound as a white solid (3.5 g, 49.8%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08071581B2 |
| 출처 데이터셋 | uspto-grants-2011_12 |
| ORD ID | ord-1a35cf78a93446f093396b06b5071da6 |
| 출처 메모 | uspto-grants-2011_12 |