Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 5-Bromo-2,3-difluoropyridine | HCID 14549654 | — |
| Reactant | HCID 178507942 | HCID 178507942 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 90020871 | HCID 90020871 | 46.3% |
Reaction Steps
Mix 2-aminopyridin-4-ol (1.13 g, 10.3 mmol), 5-bromo-2,3-difluoro-pyridine (2 g, 10.3 mmol) in DMF (10 mL). Stir the mixture at 120° C. for 3 hrs. TLC (EtOAc:PE=1:1) shows the reaction is complete. Filter, add water (50 mL) to the filtrate, extract with EtOAc (50 mL×3). Combine the organic layers, dry over anhydrous Na2SO4. Concentrate to give the crude product. Purification by chromatography (silica gel, EtOAc:PE=1:4) affords the title compound (1.35 g, 46.3%). MS: (M+1): 284.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09359338B2 |
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| Source dataset | uspto-grants-2016_06 |
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| ORD ID | ord-5d8b99116ed84c34aa28c01b415d65b6 |
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| Source note | uspto-grants-2016_06 |
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