Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Cesium carbonate → 5-iodo-1-pyridin-3-yl-1H-indazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 2-Fluoro-5-iodobenzaldehyde | HCID 16217058 | — |
| 반응물 | 3-Hydrazinylpyridine dihydrochloride | HCID 17132489 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | 5-iodo-1-pyridin-3-yl-1H-indazole | HCID 59786571 | 93.9% |
반응 단계
Cesiumcarbonate (26.84 g, 82.38 mmol) is added to a suspension of 2-fluoro-5-iodobenzaldehyde (6.87 g, 27.46 mmol) and 3-pyridylhydrazine dihydrochloride (5 g, 27.46 mmol) in 136 mL N-methylpyrrolidon. The reaction mixture is stirred overnight at room temperature. After checking that the hydrazone has been formed (1H-NMR) the reaction mixture is heated for four hours at 160° C. The reaction mixture is allowed to cool down and the dark brown suspension is poured on 1000 mL ice water. After vigorously stirring at room temperature for 45 minutes, the precipitated product is sucked off via a glass microfibre filter, washed with water and dried at the evaporator at 45° C. 8.28 g (93.9%) of the title compound are obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08030340B2 |
| 출처 데이터셋 | uspto-grants-2011_10 |
| ORD ID | ord-5caddc39b2ab4bffb3eda6ad13631f43 |
| 출처 메모 | uspto-grants-2011_10 |