Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → 4-Bromo-6-chloro-2-methyl-2,3-dihydropyridazin-3-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 4-Bromo-6-chloro-2,3-dihydropyridazin-3-one | HCID 11586522 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4-Bromo-6-chloro-2-methyl-2,3-dihydropyridazin-3-one | HCID 59216474 | 97.5% |
반응 단계
4-Bromo-6-chloro-2H-pyridazin-3-one (5.02 g, 23.97 mmol) was dissolved in 40 ml dimethylformamide. Cesium carbonate (9.37 g, 28.76 mmol) was added. After 5 min, iodomethane (5.103 g, 35.95 mmol) was added dropwise over 20 min. The reaction mixture was stirred 3 hours at room temperature. The precipitate was filtered off and concentrated and the resulting residue was treated with 20 ml dichloromethane. The insoluble material was filtered off again and washed with dichloromethane. The filtrate was concentrated in vacuo to yield 4-Bromo-6-chloro-2-methyl-2H-pyridazine-3-one (5.223 g, 23.37 mmol). MS (ESI) 224.9 (M+H)+
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08822457B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-4716460160e64d4f9fd22f14877dfffc |
| 출처 메모 | uspto-grants-2014_09 |