Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-((6-methylpyridin-2-yl)methyl)-4-nitro-3-vinyl-1H-indazole → 3-ethyl-((6-methylpyridin-2-yl)methyl)-1H-indazol-4-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-((6-methylpyridin-2-yl)methyl)-4-nitro-3-vinyl-1H-indazole | HCID 67259703 | — |
| 촉매 | Palladium hydroxide | HCID 9942167 | — |
| 용매 | Dichloromethane ethanol | HCID 21584144 | — |
| 생성물 | 3-ethyl-((6-methylpyridin-2-yl)methyl)-1H-indazol-4-amine | HCID 67259804 | 87.8% |
반응 단계
To 1-((6-methylpyridin-2-yl)methyl)-4-nitro-3-vinyl-1H-indazole (28.2 g, 95.8 mmol, Example 5, step C) in EtOH/DCM (300 mL/10 mL) was added palladium hydroxide (15 g, 20% wt). The reaction was purged with N2 and charged with hydrogen to 45 psi. The reaction was recharged during the reaction to 45 psi 4-5 times for the first 30 minutes. After 2 hours, the reaction was stopped, filtered through Celite, and the filter pad was washed with MeOH/DCM/Et3N (1 L, 10:1:1). The filtrate was concentrated and silica gel chromatography (EtOAc/hexanes 1:3) to provide the desired product (22.4 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08841455B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-a4f5e7c48c9143ab82cd155c46a4ec4b |
| 출처 메모 | uspto-grants-2014_09 |