Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethyl 2-cyano-3-ethoxy-2-butenoate → Ethyl 7-amino-mesityl-2,5-dimethylpyrazolo[1,5-a]pyrimidin-6-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethyl 2-cyano-3-ethoxy-2-butenoate | HCID 46635 | — |
| 반응물 | HCID 178424562 | HCID 178424562 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | Ethyl 7-amino-mesityl-2,5-dimethylpyrazolo[1,5-a]pyrimidin-6-carboxylate | HCID 22249773 | 20.4% |
반응 단계
Concentrated dihydrochloric acid (0.1 mL) was added to a solution of 4-mesityl-3-methyl-1H-5-pyrazoleamine (2.5 g, 11.61 mmol) and ethyl 2-cyano-3-ethoxy-2-butenoate (2.13 g, 11.61 mmol) in ethanol (30 mL), followed by heating under reflux for 18 hours. The reaction mixture was evaporated as it was. Then, water was added and a 5N aqueous solution of sodium hydroxide was added under ice-cooling, to neutralize. Further, the mixture was extracted with ethyl acetate, and the organic layer was washed with brine, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography (15% ethyl acetate/hexane), to give the title compound (835 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06995163B2 |
| 출처 데이터셋 | uspto-grants-2006_02 |
| ORD ID | ord-136303b2067444509e1f937d0012b62a |
| 출처 메모 | uspto-grants-2006_02 |