Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzonitrile | HCID 7505 | — |
| Reactant | 1,10-Phenanthroline hydrate | HCID 21226 | — |
| Reactant | 2-Amino-5-bromopyridine | HCID 70622 | — |
| Catalyst | copper(I) bromide | HCID 24593 | — |
| Product | HCID 71680411 | HCID 71680411 | 38% |
Reaction Steps
A mixture of 5-bromopyridin-2-amine (2 g, 11.6 mmol), benzonitrile (26.2 g, 26.1 ml, 254 mmol), 1,10-phenanthroline monohydrate (115 mg, 578 μmol) and copper (I) bromide (82.9 mg, 578 μmol) was placed in a 100 ml 2 necked flask. The mixture was heated to 135° C. while air was bubbled gently through the mixture for 2 days. Another portion of copper (I) bromide (82.9 mg, 578 μmol) and 1,10-phenanthroline monohydrate (115 mg, 578 μmol) was added and bubbling and heating was continued for further 8 hours. The solvent was evaporated. Purification by flash chromatography on a 20 g silicagel column using heptane/ethyl acetate 10-50% as eluent and evaporation of the solvents afforded 6-bromo-2-phenyl-[1,2,4]triazolo[1,5-a]pyridine (1.19 g, 38%) as light yellow solid. Mp.: 146° C. MS: m/z=274/276 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09227970B2 |
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| Source dataset | uspto-grants-2016_01 |
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| ORD ID | ord-99dd94ee27e746178fcaf149a6a59bc8 |
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| Source note | uspto-grants-2016_01 |
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