HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 4-Boc-1-(5-bromo-2-pyridyl)piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Reactant | 5-Bromo-2-fluoropyridine | HCID 2783168 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-Boc-1-(5-bromo-2-pyridyl)piperazine | HCID 11244775 | 37.4% |
Reaction Conditions
| Temperature | 130 °C |
|---|
Reaction Steps
5-Bromo-2-fluoropyridine (3.0 g) was dissolved in DMF (18 ml), and K2CO3 (1.31 g) and tert-butyl piperazine-1-carboxylate (1.76 g) were added thereto, followed by stirring at 130° C. for 3 days. The reaction mixture was concentrated under reduced pressure, and then a saturated aqueous sodium hydrogen carbonate solution was added thereto, followed by extraction with CHCl3. The organic layer was dried over Na2SO4 and the solvent was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/EtOAc) to obtain tert-butyl 4-(5-bromopyridin-2-yl)piperazine-1-carboxylate (1.21 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08802679B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-74479b55d24d4a50b6a7ec2930dd5bb3 |
| Source note | uspto-grants-2014_08 |