Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Trifluoroacetic anhydride | HCID 9845 | — |
| Reactant | HCID 178513505 | HCID 178513505 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178509428 | HCID 178509428 | 14.1% |
Reaction Steps
To a mixture of 22 mg (0.05 mmol) of 5-(4-benzyloxy-phenyl)-6-cyclohexyl-7-oxo-4,7-dihydro-pyrazolo[1,5-a]pyrimidine-2-carboxylic acid amide in 1 mL of dichloromethane (DCM) was added 0.04 mL (0.3 mmol) of triethylamine (Et3N), and the resulting mixture was cooled in an ice bath. Then 0.021 mL (0.15 mmol) of trifluoroacetic anhydride ((CF3CO)2O) was added during which time the mixture became homogeneous, and was stirred for 2.5 h. The reaction mixture was quenched by the addition of water, and concentrated to a residue which was purified via reverse-phase chromatography to afford (after lyophilization) 3 mg (14% yield) of desired 5-(4-benzyloxy-phenyl)-6-cyclohexyl-7-oxo-4,7-dihydro-pyrazolo[1,5-a]pyrimidine-2-carbonitrile as indicated by LC-MS calcd for C26H24N4O2 [M++H]+: 425.19, found: 425.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07196111B2 |
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| Source dataset | uspto-grants-2007_03 |
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| ORD ID | ord-ad6ae84c2c0c4d3697fb8c5ce9c9e148 |
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| Source note | uspto-grants-2007_03 |
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