Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Chloride | HCID 312 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | 2,5-Dibromopyridine | HCID 69353 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Product | 5-Bromo-2-cyclopropylpyridine | HCID 22317722 | 103% |
Reaction Steps
To a solution 2,5-dibromopyridine [CAS 624-28-2, commercially available] (5 g, 21 mmol) and Pd(PPh3)4 (244 mg, 1 mol %) in THF (25 mL) was added cycloropylzinc chloride (0.4M in THF, 53 mL, 26 mmol), and the mixture was stirred under argon atmosphere at 70° C. for 3 h. Cooled to 23° C., poured into sat. NaHCO3-solution, extracted with ether, washed with brine, dried over Na2SO4. Removal of the solvent in vacuum left a brown oil, which was purified by silica gel chromatography with heptane-EtOAc (9:1) to give the title compound as a colorless liquid (4.3 g, 103%). MS (EI) 197 [(M)+] and 199 [(M+2)+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08063048B2 |
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| Source dataset | uspto-grants-2011_11 |
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| ORD ID | ord-46623bb598c9461087a3b866c2491683 |
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| Source note | uspto-grants-2011_11 |
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