HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → Ammonia
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | 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 | — |
| Katalysator | Methanol | HCID 887 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | Ammonia | HCID 222 | 5% |
| Produkt | HCID 68905815 | HCID 68905815 | — |
Reaktionsschritte
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]−.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07582631B2 |
| Quelldatensatz | uspto-grants-2009_09 |
| ORD ID | ord-2628d9afc08144469b329a41aee971d3 |
| Quellennotiz | uspto-grants-2009_09 |