HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178509821, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 178453058 | HCID 178453058 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178509821 | HCID 178509821 | 88.8% |
Reaction Steps
A mixture of N-{2,4-dichloro-3-[6-(trans-4-trifluoromethyl-cyclohexylcarbamoyl)-5-(2,2-difluoro-ethoxy)-3H-imidazo[4,5-b]pyridin-2-ylamino]benzyl}-carbamic acid tert-butyl ester (6.3 g, 9.3 mmol), 4 M HCl in dioxane (60 ml) and MeOH (5 ml) is stirred for 15 min. The mixture is concentrated, diluted with water and basified with conc. NH3. The precipitate is collected by filtration, washed with water, dried and purified via prep HPLC. The product fractions are concentrated, basified with conc. NH3, extracted with EtOAc. The organic phases are dried with Na2SO4 and concentrated to give the crude sub-title compound (4.8 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08586604B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-082b7e34eb5a49d18c0c6cea6a4b60e6 |
| Source note | uspto-grants-2013_11 |