Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 3-[2-{(1R*,2R*)-2-hydroxy-2-methylcyclohexyl}-3-oxo-2,3-dihydropyridazin-6-yl]-2-phenylpyrazolo[1,5-a]-pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 1-Methyl-1,2-epoxycyclohexane | HCID 224243 | — |
| 반응물 | 3(2H)-Pyridazinone, 6-(2-phenylpyrazolo[1,5-a]pyridin-3-yl)- | HCID 10589418 | — |
| 촉매 | Benzyltrimethylammonium chloride | HCID 5963 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 3-[2-{(1R*,2R*)-2-hydroxy-2-methylcyclohexyl}-3-oxo-2,3-dihydropyridazin-6-yl]-2-phenylpyrazolo[1,5-a]-pyridine | HCID 70157518 | 6% |
반응 단계
A mixture of 3-(3-oxo-2,3-dihydropyridazin-6-yl)-2-phenylpyrazolo[1,5-a]pyridine (2.25 g), 1-methyl-1,2-epoxycyclohexane (1.31 g), benzyltrimethylammonium chloride (178 mg), 1N aqueous sodium hydroxide (7.8 ml), water (17 ml), and toluene was heated to reflux for 8 hours and 20 minutes. After the reaction mixture was cooled to room temperature, the precipitates were collected by filtration, washed with water, and dried. The crude material was purified by column chromatography on silica gel (CH2Cl2:EtOAc=10:2) to give colorless crystals of 3-[2-{(1R*,2R*)-2-hydroxy-2-methylcyclohexyl}-3-oxo-2,3-dihydropyridazin-6-yl]-2-phenylpyrazolo[1,5-a]-pyridine (189 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06355640B1 |
| 출처 데이터셋 | uspto-grants-2002_03 |
| ORD ID | ord-b20287faa830487eb32ce42fa4bd440f |
| 출처 메모 | uspto-grants-2002_03 |