Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dichloromethane → 4-[1-(2,2-Difluoroethyl)-3-iodo-1H-pyrazol-4-yl]-2-(methylthio)pyrimidine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1,1-Difluoro-2-iodoethane | HCID 3833565 | — |
| 반응물 | 4-(5-Iodo-1H-pyrazol-4-yl)-2-(methylsulfanyl)pyrimidine | HCID 46864160 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4-[1-(2,2-Difluoroethyl)-3-iodo-1H-pyrazol-4-yl]-2-(methylthio)pyrimidine | HCID 57856303 | — |
반응 단계
To a solution of Intermediate A (83 g, 0.26 mol) in DMF (600 mL) were K2CO3 (58 g, 0.417 mol) and 1,1-difluoro-2-iodo-ethane (60 g, 0.313 mol). Then the mixture was stirred at room temperature overnight. TLC (CH2Cl2: MeOH=20:1) showed the reaction was complete. The mixture was concentrated and the solid was diluted with CH2Cl2 (500 mL). The slurry was filtered and the filtrate was concentrated to give crude product, which was purified via prep. SFC to give compound B-33-1 (41.1 g, 41.3%) as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07772246B2 |
| 출처 데이터셋 | uspto-grants-2010_08 |
| ORD ID | ord-9295e04992444ecf89f3017e5d1f211e |
| 출처 메모 | uspto-grants-2010_08 |