Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diethyl Ether → 3-tert-Butoxy-5-fluoropyrazine-2-carboxaldehyde
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diethyl Ether | HCID 3283 | — |
| 반응물 | 18-Crown-6 | HCID 28557 | — |
| 반응물 | Potassium Fluoride | HCID 522689 | — |
| 반응물 | 3-Tert-butoxy-5-chloropyrazine-2-carboxaldehyde | HCID 22248202 | — |
| 촉매 | Tetraphenylphosphonium Bromide | HCID 2724163 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 3-tert-Butoxy-5-fluoropyrazine-2-carboxaldehyde | HCID 22248252 | 3.4% |
반응 단계
After dissolving 5.86 g of the crude 3-tert-butoxy-5-chloropyrazine-2-carboxaldehyde in 55 ml of acetonitrile, 4.77 g of potassium fluoride, 1.13 g of tetraphenylphosphonium bromide and 0.71 g of 18-crown-6 were added and the mixture was heated to reflux for 4 hours. Diethyl ether was added to the reaction mixture, the insoluble portion was filtered out, and the filtrate was distilled off under reduced pressure. Ethyl acetate was added to the residue, the insoluble portion was filtered out, and the filtrate was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (solvent: toluene/ethyl acetate) to obtain the title compound (183 mg, 3% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07915274B2 |
| 출처 데이터셋 | uspto-grants-2011_03 |
| ORD ID | ord-770ff0fc104f4f0d81c830c87f9b527d |
| 출처 메모 | uspto-grants-2011_03 |