Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Phosphorus oxychloride → 4,5-Dichloro-6-methylpyrimidine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 5-chloro-6-methyl-1H-pyrimidin-4-one | HCID 178433212 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 4,5-Dichloro-6-methylpyrimidine | HCID 11789537 | — |
반응 단계
50 ml of POCl3 was added dropwise to a solution of 14.5 g (0.1 mol) of 4-hydroxyl-5-chloro-6-methylpyrimidine in 50 mL of toluene, the mixture was refluxed for 5-7 h after addition. After the reaction was over by Thin-Layer Chromatography monitoring, the reaction mixture was concentrated under reduced pressure to remove toluene and extra POCl3, and then poured into ice water. The water phase was extracted with ethyl acetate (3×50 ml), the organic phases were emerged, dried over anhydrous magnesium sulfate, filtered and then concentrated under reduced pressure. The residue was purified through silica column to give 14.43 g as yellow liquid with yield of 88.5%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09447081B2 |
| 출처 데이터셋 | uspto-grants-2016_09 |
| ORD ID | ord-acc06ae59eee41788d3bed827fd3e2f3 |
| 출처 메모 | uspto-grants-2016_09 |