Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pyridine → 5-{2-[2-Chloro-4-(4-fluoro-3-methoxy-phenoxy)-phenyl]-1-hydroxy-1-trifluoromethyl-propyl}-1-methyl-1H-pyridin-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | (4-Fluoro-3-methoxyphenyl)boronic acid | HCID 44558185 | — |
| 반응물 | 5-[2-(2-Chloro-4-hydroxy-phenyl)-1-hydroxy-1-trifluoromethyl-propyl]-1-methyl-1H-pyridin-2-one | HCID 57421314 | — |
| 촉매 | Cupric acetate | HCID 8895 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 5-{2-[2-Chloro-4-(4-fluoro-3-methoxy-phenoxy)-phenyl]-1-hydroxy-1-trifluoromethyl-propyl}-1-methyl-1H-pyridin-2-one | HCID 57421316 | 51.7% |
반응 단계
To a solution of 5-[2-(2-chloro-4-hydroxy-phenyl)-1-hydroxy-1-trifluoromethyl-propyl]-1-methyl-1H-pyridin-2-one (Example 196, 200 mg) in CH2Cl2 (4 ml) were added 4-fluoro-3-methoxyphenylboronic acid (282 mg), copper-(II)-acetate (307 mg), molecular sieve and pyridine (219 mg). The mixture was stirred at room temperature under an air atmosphere with exclusion of moisture for 7 days. The mixture was filtered, diluted with CH2Cl2 and washed with 1M aqueous HCl. The organic phase was dried (MgSO4), filtered and concentrated to dryness. The product was purified by chromatography (SiO2, cyclohexane/EtOAc 1:0=>0:1) to give the title compound (139 mg) as an off-white solid. MS (m/e)=486.3 [M+H+].
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08883786B2 |
| 출처 데이터셋 | uspto-grants-2014_11 |
| ORD ID | ord-1022c9cfb3b3434f9a2212bd4e65af53 |
| 출처 메모 | uspto-grants-2014_11 |