Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diethyl Ether → 1-(3,5-Dichloro-2-pyridyl)-3-trifluoromethylpropane-1,3-dione
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diethyl Ether | HCID 3283 | — |
| 반응물 | 2,2,2-Trifluoroethyl Acetate | HCID 136256 | — |
| 반응물 | Sodium ethoxide | HCID 2723922 | — |
| 반응물 | 1-(3,5-Dichloropyridin-2-yl)ethanone | HCID 21712163 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 1-(3,5-Dichloro-2-pyridyl)-3-trifluoromethylpropane-1,3-dione | HCID 21712152 | — |
반응 단계
15.8 g of 3,5-dichloro-2-acetylpyridine are introduced together with 12.0 ml of trifluoroethyl acetate into 125 ml of absolute ether. With stirring, the mixture is cooled using an ice-bath and 46.6 ml of, a 21% sodium ethanolate solution in ethanol are added dropwise. The ice-bath is then removed and the mixture is subsequently stirred overnight at 25° C. After cooling the reaction mixture in an ice-bath and adding dropwise 7.5 ml of glacial acetic acid, the mixture is concentrated in vacuo. 39.0 g of 1-(3,5-dichloro-2-pyridyl)-3-trifluoromethylpropane-1,3-dione are obtained, which can be used directly for the following cyclisation step.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06274536B1 |
| 출처 데이터셋 | uspto-grants-2001_08 |
| ORD ID | ord-d48b8b86d8ba4b78b29c8927f41d80b5 |
| 출처 메모 | uspto-grants-2001_08 |