Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Potassium Acetate | HCID 517044 | — |
| Reactant | 2-Fluorophenylboronic acid | HCID 2734354 | — |
| Reactant | HCID 86680089 | HCID 86680089 | — |
| Catalyst | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 86680088 | HCID 86680088 | 33% |
Reaction Steps
Following the procedures of Examples 101 or 112, (R)-3-amino-6-bromo-N-(1-(2,2-difluoroethyl)-5-(4-(2,2,2-trifluoroacetamido)azepan-1-yl)-1H-pyrazol-4-yl)picolinamide was prepared. In a microwave reaction tube, (R)-3-amino-6-bromo-N-(1-(2,2-difluoroethyl)-5-(4-(2,2,2-trifluoroacetamido)azepan-1-yl)-1H-pyrazol-4-yl)picolinamide (284 mg, 0.51 mmol), (2-fluorophenyl)boronic acid (215 mg, 1.54 mmol), and Pd(dppf)2Cl2 (37 mg, 0.051 mmol) were dissolved in acetonitrile (4 mL). 1.0M potassium acetate (0.77 mL, 0.77 mmol) and 1.0 M sodium carbonate (0.77 mL, 0.77 mmol) were added. The mixture was irradiated under microwave at 120° C. for 30 min. It was cooled and filtered through Celite and washed with methanol. The filtrate was concentrated and purified by flash chromatography eluting with 0 to 10% methanol in methylene chloride to give (R)-3-amino-N-(1-(2,2-difluoroethyl)-5-(4-(2,2,2-trifluoroacetamido)azepan-1-yl)-1H-pyrazol-4-yl)-6-(2-fluorophenyl)picolinamide (98 mg, 33%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08614206B2 |
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| Source dataset | uspto-grants-2013_12 |
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| ORD ID | ord-42172b981cc747fa84f195be8b1ee3e5 |
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| Source note | uspto-grants-2013_12 |
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