Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Carbonate → 5-(2-Fluoro-5-methylpyridin-3-yl)-2,4-dimethoxy-pyrimidine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | (2,4-Dimethoxypyrimidin-5-yl)boronic acid | HCID 2736209 | — |
| 반응물 | 3-Bromo-2-fluoro-5-methylpyridine | HCID 21816563 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | 1-Propanol | HCID 1031 | — |
| 생성물 | 5-(2-Fluoro-5-methylpyridin-3-yl)-2,4-dimethoxy-pyrimidine | HCID 58994169 | 33.4% |
반응 단계
2,4-Dimethoxy-pyrimidine-5-boronic acid (842 mg, 4.60 mmol) was dissolved in degassed n-PrOH (55 ml) and then 2-fluoro-3-bromo-5-methylpyridine (800 mg, 4.21 mmol), Na2CO3 (1.46 g, 13.77 mmol), PPh3 (348 mg, 1.33 mmol) and Pd(OAc)2 (101 mg, 0.45 mmol) were added. The suspension was stirred at reflux for 2 hours. After cooling, the solvent was evaporated under vacuum and the crude was partitioned between water and ethyl acetate. The organic phase was dried (Na2SO4) and evaporated. The residue was triturated with Et2O to give 350 mg of the title compound as a gray powder (31% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07727988B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-12f4a5822159455fbcc84489de49ee47 |
| 출처 메모 | uspto-grants-2010_06 |