Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → 6-chloro-7-methylsulfanyl-3-trifluoromethyl-1H-quinoxalin-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | 4-Chloro-5-fluoro-1,2-phenylenediamine | HCID 735773 | — |
| 반응물 | Ethyl 3,3,3-trifluoro-2-oxopropanoate | HCID 2737239 | — |
| 반응물 | Sodium hydrogen sulfide hydrate | HCID 53442613 | — |
| 반응물 | HCID 178517239 | HCID 178517239 | — |
| 반응물 | HCID 178517316 | HCID 178517316 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 6-chloro-7-methylsulfanyl-3-trifluoromethyl-1H-quinoxalin-2-one | HCID 22341150 | 38% |
반응 단계
A mixture of 6-chloro-7-fluoro-3-trifluoromethyl-quinoxalin-2-ol and 7-chloro-6-fluoro-3-trifluoromethyl-quinoxalin-2-ol (4.1 g, prepared similarly as described above from 4-chloro-5fluoro-1,2-diaminobenzene and ethyl trifluoropyruvate) was dissolved in DMF (140 ml) and sodium hydrogen sulfide monohydrate (3.5 g, 47 mmol) was added. The reaction mixture was stirred at room temperature for 1 hour and then iodomethane (3.5 ml) was added. Stirring was continued for 10 minutes and the reaction mixture was poured on ice/water (500 ml). The separated crystals were filtered, dried and recrystallised from ethanol to afford 1.73 g (38%) of 6-chloro-7-methylsulfanyl-3-trifluoromethyl-1H-quinoxalin-2-one.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06927214B1 |
| 출처 데이터셋 | uspto-grants-2005_08 |
| ORD ID | ord-6c0033fd1fff4e99a6ba8ec915762f25 |
| 출처 메모 | uspto-grants-2005_08 |