HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 56646040, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 66665999 | HCID 66665999 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 56646040 | HCID 56646040 | 7.3% |
Reaction Steps
To a mixture of crude {1-[4-(3-phenyl-imidazo[1,2-a]pyrimidin-2-yl)-phenyl]-cyclobutyl}-carbamic acid tert-butyl ester (390 mg) in DCM (0.9 mL) and methanol (0.57 mL) was added a solution of 4 M hydrogen chloride in dioxane (1.77 mL) and the mixture was stirred overnight at rt. The mixture was poured onto ice, made alkaline with aqueous sodium hydroxide (2 N) and extracted three times with a mixture of DCM/methanol. The combined organic phases were washed with brine, dried and concentrated in vacuo to give the crude title compound as a yellow oil. Purification was achieved by chromatography [amino phase silica; gradient elution: hexane to EtOAc], followed by trituration with diisopropylether at 0° C. to give the title compound (21.9 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08975265B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-c827a01413bb46aea6d83b7ecf851503 |
| Source note | uspto-grants-2015_03 |