Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Phosphorus oxychloride → 2,6-Dichloro-4-methylpyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 2-Chloro-4-methylpyridine 1-oxide | HCID 12487484 | — |
| 생성물 | 2,6-Dichloro-4-methylpyridine | HCID 10898997 | 43% |
반응 단계
A mixture of 2-chloro-4-methyl-pyridine 1-oxide (1.0 g, 7.0 mmol) and phosphorus oxychloride (10 mL) was heated at reflux for 4 h. The volatiles were evaporated and the residue dissolved in ethyl acetate. The solution was washed with ice-water followed by sodium bicarbonate solution. The organic phase was again washed with water, brine solution, dried over anhydrous sodium sulfate and concentrated to obtain a residue which was purified by column chromatography over silica gel (60-120 mesh) using petroleum ether as eluent to afford 2,6-dichloro-4-methyl-pyridine (491 mg, 43%) as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08524705B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-51cb4aae7be0496d84ff01fb90662113 |
| 출처 메모 | uspto-grants-2013_09 |