Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 1-Methyl-4-nitro-1H-indazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 4-Nitroindazole | HCID 18057 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-Methyl-4-nitro-1H-indazole | HCID 280213 | 35.3% |
반응 단계
6.5 g of 4-nitroindazole (Chem. Ber. (1904), 37, 2583), 1.9 ml of methyl iodide and 14.4 g of cesium carbonate in 110 ml of DMF are stirred for 2 hours at 0° C. and then for 12 hours at room temperature. It is added to water and extracted with ethyl acetate. The organic phase is washed with water and brine, dried (Na2SO4) and concentrated by evaporation. The residue is recrystallized from ethyl acetate/hexane. 2.49 g of 1-methyl-4-nitroindazole is obtained. The latter is hydrogenated in 70 ml of THF with 420 mg of palladium on activated carbon under normal pressure with hydrogen. The batch is filtered through diatomaceous earth and completely concentrated by evaporation. 2.1 g of the title compound is obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07659297B2 |
| 출처 데이터셋 | uspto-grants-2010_02 |
| ORD ID | ord-448ff966a4e34c64a3d0687be6454d6e |
| 출처 메모 | uspto-grants-2010_02 |