Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → Ammonia
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 5-{1-[2-(1-phenyl-ethylamino)-pyridin-4-yl]-1H-indazol-3-yl}-2,5-diaza-bicyclo[2.2.1]heptane-2-carboxylic acid tert-butyl ester | HCID 68910731 | — |
| 촉매 | Methanol | HCID 887 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | Ammonia | HCID 222 | 5% |
| 생성물 | HCID 68905815 | HCID 68905815 | — |
반응 단계
To the 5-{1-[2-(1-phenyl-ethylamino)-pyridin-4-yl]-1H-indazol-3-yl}-2,5-diaza-bicyclo[2.2.1]heptane-2-carboxylic acid tert-butyl ester (0.044 g, 0.086 mmol) were added 4N HCl in dioxane (1 mL) and a few drops of methanol. After stirring at room temperature for 30 min, the reaction was concentrated in vacuo and the residue was partitioned between methylene chloride and saturated sodium bicarbonate; the aqueous layer was back-extracted with methylene chloride (2×). The combined organic extract was dried (K2CO3), filtered, and concentrated in vacuo. Flash chromatography with 1%, 3%, and 5% 2M NH3 in MeOH/CHCl3 gave the title compound as a cream colored solid. MS (ES+): 411.3 [M+H]+, 409.5 [M−H]−.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07582631B2 |
| 출처 데이터셋 | uspto-grants-2009_09 |
| ORD ID | ord-2628d9afc08144469b329a41aee971d3 |
| 출처 메모 | uspto-grants-2009_09 |