Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → Ethyl 2,4-dichloro-5-fluorobenzoylacetate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Diethyl Carbonate | HCID 7766 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Acetophenone, 2',4'-dichloro-5'-fluoro- | HCID 727250 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | Ethyl 2,4-dichloro-5-fluorobenzoylacetate | HCID 2774350 | 45% |
반응 단계
To a suspension of prewashed sodium hydride (76.8 g) in ether was added 189 g of diethylcarbonate. The mixture was heated to reflux and a solution of 131.84 g of 6-acetyl-1,3-dichloro-4-fluorobenzene in 1500 ml of ether was added dropwise over 5 hours. The mixture was then refluxed 24 hours, cooled, poured onto a mixture of ice and acetic acid and extracted several times with ether. The ether extracts were combined, washed with water, dried and evaporated. The residue was purified by vacuum distillation giving 80 g of ethyl 2,4-dichloro-5-fluorobenzoylacetate.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05210193 |
| 출처 데이터셋 | uspto-grants-1993_05 |
| ORD ID | ord-27c25f8a47ee49479ecdd224e997d1c6 |
| 출처 메모 | uspto-grants-1993_05 |