HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 1-(2-Pyridyl)piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2,3-Dichloropyridine | HCID 16988 | — |
| Reactant | 2-Methylpiperazine, (S)- | HCID 2734219 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | 1-(2-Pyridyl)piperazine | HCID 94459 | — |
Reaction Steps
Dissolve 2,3-dichloropyridine (7.4 g, 0.05 moles) and (S)-(−)-2-methylpiperazine (5.0 g, 0.05 moles) in DMA (125.0 mL) under nitrogen atmosphere. Add anhydrous powdered K2CO3 (20.75 g, 0.15 moles) to this mixture and stir at 135-140° C. for 56 hours. Cool the reaction mixture to room temperature, dilute with water (400 mL), extract with EtOAc (3×200 mL) and wash the combined organic extract with brine (2×150 mL). Dry over MgSO4, and concentrate under vacuum to afford crude product as yellow liquid. Purify by flash column chromatography using CHCl3 to afford pyridylpiperazine derivative as yellow viscous oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07566712B2 |
| Source dataset | uspto-grants-2009_07 |
| ORD ID | ord-e02010b6877f430cb3d58b1d391b7b0e |
| Source note | uspto-grants-2009_07 |