Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Phosphorus oxychloride → 2-Chloro-4-(4-trifluoromethylphenyl)pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 4-(4-(Trifluoromethyl)phenyl)pyridine 1-oxide | HCID 57350829 | — |
| 생성물 | 2-Chloro-4-(4-trifluoromethylphenyl)pyridine | HCID 28875863 | — |
반응 단계
To 4-(4-trifluoromethyl-phenyl)-pyridine 1-oxide (2.4 g, 10 mmol) was added phosphorous oxychloride (12 mL) at room temperature. The reaction mixture was heated at reflux for 5 h. POCl3 was removed under reduced pressure, and the residue was partitioned between EtOAc and aqueous ammonium hydroxide. The aqueous layer was extracted with EtOAc and the combined organic layers were dried over Na2SO4, filtered, and concentrated in vacuo. The crude material was purified by chromatography on a Biotage 40 M column (8:1 hexanes:EtOAc) to give the title compound as a white solid. MS (ESI, pos. ion) m/z: 258.5 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07582657B2 |
| 출처 데이터셋 | uspto-grants-2009_09 |
| ORD ID | ord-b9880877cfc945ae9dd7d354a2c150a8 |
| 출처 메모 | uspto-grants-2009_09 |