Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | 3-[4-(1-Amino-cyclobutyl)-phenyl]-6-fluoro-2-phenyl-chromen-4-one | HCID 51030598 | — |
| Reactant | HCID 67067748 | HCID 67067748 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 67067844 | HCID 67067844 | 65% |
Reaction Steps
Following the procedure of 3-[4-(1-amino-cyclobutyl)-phenyl]-6-fluoro-2-phenyl-chromen-4-one, (1-{4-[8-(1,5-dimethyl-1H-pyrazol-4-yl)-4-oxo-2-phenyl-4H-chromen-3-yl]-phenyl}-cyclobutyl)-carbamic acid tert-butyl ester was treated with TFA. The resultant free base was dissolved in a mixture of MeOH (7 mL), water (7 mL) and 1 M HCl (0.6 mL) and chromatographed on a 5 g C18 cartridge {gradient 10 to 50% MeOH in water+1 M HCl (60 μL in each 10 mL of eluent)} to give the title compound as a white solid (23 mg, 65%). 1H NMR (400 MHz, DMSO-d6): δ 8.61 (s, 3H), 8.01 (dd, J=7.9 and 1.7 Hz, 1H), 7.71 (dd, J=7.3 and 1.6 Hz, 1H), 7.67 (s, 1H), 7.53 (t, J=7.6 Hz, 1H), 7.42 (d, J=8.4 Hz, 2H), 7.37-7.22 (m, 7H), 3.74 (s, 3H), 2.57-2.43 (m, 4H), 2.22 (s, 3H), 2.19-2.05 (m, 1H), 1.81-1.69 (m, 1H). LCMS (Method E): RT=3.29 min, [M+H]+=462.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08546376B2 |
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| Source dataset | uspto-grants-2013_10 |
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| ORD ID | ord-6c0c4493c7e34761ba139e29e4599500 |
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| Source note | uspto-grants-2013_10 |
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