Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sulfuric Acid → HCID 178469635, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Potassium 2-chloro-3-ethoxy-3-oxoprop-1-en-1-olate | HCID 74089075 | — |
| 반응물 | HCID 178507942 | HCID 178507942 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | HCID 178469635 | HCID 178469635 | 14.9% |
반응 단계
To a chilled (0° C.) solution of potassium 2-chloro-3-ethoxy-3-oxoprop-1-en-1-olate (16.4 g, 86.3 mmol) in concentrated sulfuric acid (43.5 mmol) and ethanol (50 mL) was added 2-aminopyridin-4-ol (3 g, 27 mmol). The resulting mixture was warmed to ambient temperature and refluxed for 10 hours. The reaction was concentrated and suspended in EtOAc. The solids were isolated to afford 829 mg of pure product. The supernatant was concentrated, and subjected to chromatography on silica with 30% EtOAc/Hexanes as eluent to afford a second batch of desired product (5.8 g, 80% purity) as a brown, viscous oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09174981B2 |
| 출처 데이터셋 | uspto-grants-2015_11 |
| ORD ID | ord-1a02d7f524eb42f692196d702fb7dcce |
| 출처 메모 | uspto-grants-2015_11 |