Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pyridine → Ethyl 3-(2-phenyl-1-cyclopropyl)-3-oxo-propanoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | 2,2-Dimethyl-1,3-dioxane-4,6-dione | HCID 16249 | — |
| 반응물 | Cyclopropanecarbonyl chloride, 2-phenyl- | HCID 523092 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Ethyl 3-(2-phenyl-1-cyclopropyl)-3-oxo-propanoate | HCID 20034593 | 108.9% |
반응 단계
A solution of 2-phenyl-1-cyclopropanecarboxylic acid chloride (15 g) in 1,2-dichloroethane (70 ml) is added at 0° C. to a solution of 2,2-dimethyl-1,3-dioxane-4,6-dione (Meldrum's acid, 12 g) and pyridine (13.2 g) in 1,2-dichloroethane (70 ml) and the solution is stirred at room temperature for one hour. A 2N water solution of H2SO4 (20 ml) is then added, the two layers are separated and the organic phase is washed twice with water (50 ml), dryed on Na2SO4 and evaporated in vacuum. The residue is dissolved in EtOH (150 ml), heated to the reflux temperature for two hours and evaporated to dryness to give almost pure ethyl 3-(2-phenyl-1-cyclopropyl)-3-oxo-propanoate (21 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04845113 |
| 출처 데이터셋 | uspto-grants-1989_07 |
| ORD ID | ord-7865c18e0e4847a6b3d2252f1c412f04 |
| 출처 메모 | uspto-grants-1989_07 |