HuagongsheHuagongshe Chemistry Print Report · For research reference only
Piperazine → HCID 5255691, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 10778001 | HCID 10778001 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 5255691 | HCID 5255691 | — |
Reaction Steps
To a mixture of 10.0 g (37.9 mmol) of 8,11-dichloro-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridine and 1.0 m/of Et3N in 200 mL of dry THF at room temperature and under a nitrogen atmosphere was added 33.0 g of piperazine. The mixture was stirred at room temperature for 22.5 hours and then refluxed for 5.5 hours. It was then cooled to room temperature, poured into 250 mL of 5% aqueous NaOH, and extracted with CH2Cl2 (3X). The combined organic portions were washed with brine, dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified via flash chromatography (2→5% MeOH saturated with NH4OH in CH2 Cl2) to yield the title compound as a glass.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05721236 |
| Source dataset | uspto-grants-1998_02 |
| ORD ID | ord-40ac736076be4ea0a6d6c6b0ceab64d8 |
| Source note | uspto-grants-1998_02 |