Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 4-(4-Bromo-2-fluorophenylamino)-6-oxo-1-phenyl-1,6-dihydropyridazine-3-carboxylic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 4-Bromo-2-fluoroaniline | HCID 123050 | — |
| 반응물 | Methyl 4-chloro-6-oxo-1-phenyl-1,6-dihydropyridazine-3-carboxylate | HCID 2784479 | — |
| 용매 | 1,2-Dichlorobenzene | HCID 7239 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 4-(4-Bromo-2-fluorophenylamino)-6-oxo-1-phenyl-1,6-dihydropyridazine-3-carboxylic acid | HCID 66673960 | 43% |
반응 단계
To a mixture of 4-chloro-6-oxo-1-phenyl-1,6-dihydropyridazine-3-carboxylic acid methyl ester (0.250 g, 0.944 mmol) in 1,2-dichlorobenzene (3.8 mL) was added 4-bromo-2-fluoro aniline (0.561 g, 3.78 mmol), and cesium carbonate (0.615 mg, 1.89 mmol). The reaction mixture was heated to reflux. After 1 hour, the reaction mixture was cooled to room temperature. Water was added and the mixture was diluted with EtOAc. The aqueous layer was separated, acidified with 10% HCl solution, and extracted with EtOAc. The combined organic layers were dried (MgSO4), concentrated under reduced pressure, and triturated to give 0.153 g (43%) of the desired product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07732616B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-a2be2e739ec34b94a42de69e3a0075c4 |
| 출처 메모 | uspto-grants-2010_06 |