HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 56646437, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 66665421 | HCID 66665421 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 56646437 | HCID 56646437 | 50.8% |
Reaction Steps
To a mixture of crude {1-[4-(7-methoxy-3-phenyl-imidazo[1,2-a]pyrimidin-2-yl)-phenyl]-cyclobutyl}-carbamic acid tert-butyl ester (550 mg) in DCM (3 mL) and methanol (1.9 mL) was added a solution of 4 M hydrogen chloride in dioxane (5.8 mL) and the mixture was stirred for 2 hours 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. Purification was achieved by chromatography [silica; gradient elution: DCM to 8:2 DCM/ethanol] to give the title compound (220 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08975265B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-3a212a43515a42a4a61e72e654e445f9 |
| Source note | uspto-grants-2015_03 |