Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 57970097 | HCID 57970097 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Palladium | HCID 23938 | — |
| Product | HCID 57970192 | HCID 57970192 | — |
Reaction Steps
Benzyl (1-(2-(1-(2-biphenyl-2-ylacetyl)pyrrolidin-3-ylamino)quinazolin-4-yl)piperidin-3-yl)carbamate (570 mg) synthesized in the same manner as the method described in Example 1 was dissolved in methanol (6 mL), followed by addition of a solution (0.25 mL) of 4 M HCl in ethyl acetate and 10% Pd—C (100 mg), and the mixture was stirred at room temperature under hydrogen atmosphere for 3 days. The catalyst was removed by filtration, then the filtrate was concentrated, made basic with saturated aqueous sodium hydrogencarbonate, and then extracted with chloroform, and the organic layer was dried with anhydrous magnesium sulfate. The desiccant was removed by filtration, the filtrate was concentrated under reduced pressure, then the residue was purified by silica gel column chromatography (chloroform/methanol=3:1), and the resulting compound was solidified in hexane to obtain the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08044068B2 |
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| Source dataset | uspto-grants-2011_10 |
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| ORD ID | ord-285f78c42aef4832966c6b29adc5bb7e |
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| Source note | uspto-grants-2011_10 |
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