HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 66665331, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 68082624 | HCID 68082624 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Solvent | Dichloromethane methanol | HCID 21226129 | — |
| Product | HCID 66665331 | HCID 66665331 | 87.5% |
Reaction Steps
[1-(4-{7-[2-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-ethoxy]-3-phenyl-imidazo[1,2-a]pyrimidin-2-yl}-phenyl)-cyclobutyl]-carbamic acid tert-butyl ester (530 mg) was dissolved in methanol/DCM (1.3 mL/2.1 mL), treated with HCl in dioxane (4.08 mL of a 4M solution) and the mixture stirred overnight at rt. The reaction mixture was poured onto ice, made alkaline with 2N aqueous sodium hydroxide and extracted with EtOAc. The combined organic phases were washed with saturated aqueous sodium chloride, dried and concentrated in vacuo to give the crude title product as a yellow oil. Purification was achieved by trituration at 0° C. with diisopropyl ether. The resulting precipitate was filtered and dried to give the title compound as a solid (390 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08975265B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-e02a2213527e44d8aeb49e5b9debb95e |
| Source note | uspto-grants-2015_03 |