Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethyl 2-chloroacetoacetate → 5-Ethyl-2-methyl-nicotinic acid ethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethyl 2-chloroacetoacetate | HCID 11858 | — |
| 반응물 | Ethylacrolein | HCID 70203 | — |
| 반응물 | Ammonium Acetate | HCID 517165 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 5-Ethyl-2-methyl-nicotinic acid ethyl ester | HCID 14436626 | 43.2% |
반응 단계
A mixture of ethacrolein (12.8 g 0.152 mole) and ammonium acetate (24.4 g 0.304 mole) in 50 cc acetonitrile is stirred at room temperature and a solution of ethyl 2-chloroacetoacetate (25 g 0.152 mole) in 30 cc acetonitrile is added dropwise over 15 minutes. The reaction mixture is heated at reflux for 16 hours, cooled, and partitioned between water and ethyl acetate. The organic phase is concentrated in vacuo and chromatographed on silica gel using 9:1 hexane-ethylacetate to afford 12.7 g of the title product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04723011 |
| 출처 데이터셋 | uspto-grants-1988_02 |
| ORD ID | ord-24c7674dbf2448ab81e3a4fd1d43e7e8 |
| 출처 메모 | uspto-grants-1988_02 |