Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Isopropanol → 5-Ethoxycarbonyl-3-isopropoxycarbonyl-1,4-dihydro-2,6-dimethyl-4-(3-ethynylphenyl)pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Isopropanol | HCID 3776 | — |
| 반응물 | Isopropyl acetoacetate | HCID 68329 | — |
| 반응물 | 2-Butenoic acid, 3-amino-, ethyl ester, (2Z)- | HCID 643756 | — |
| 반응물 | 3-Ethynylbenzaldehyde | HCID 2771644 | — |
| 촉매 | Piperidine | HCID 8082 | — |
| 생성물 | 5-Ethoxycarbonyl-3-isopropoxycarbonyl-1,4-dihydro-2,6-dimethyl-4-(3-ethynylphenyl)pyridine | HCID 19813405 | 58.6% |
반응 단계
To a mixture of 0.65 g (0.005 mol) of 3ethynylbenzaldehyde, 1.08 g (0.0075 mol) of isopropyl acetoacetate and 25 ml of isopropyl alcohol were added 2 to 3 drops of piperidine. After heating the mixture under reflux for 24 hours, 0.65 g (0.005 mol) of ethyl 3-aminocrotonate was added thereto, further the admixture was heated under reflux for 24 hours. After completing the reaction, the reaction mixture was concentrated. The obtained precipitate was purified by subjecting to silica gel column chromatography [eluent: n-hexane to n-hexane: ethyl acetate (7 : 3)] to give 1.1 g of the desired compound (yield: 58.6%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05158963 |
| 출처 데이터셋 | uspto-grants-1992_10 |
| ORD ID | ord-d00579241cd841498e28cdd9874272dc |
| 출처 메모 | uspto-grants-1992_10 |