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 mL 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 (3×). 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 ammonia in CH2Cl2) to yield the title compound as a glass.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06365588B1 |
| Source dataset | uspto-grants-2002_04 |
| ORD ID | ord-07f5dec3ce9c4a59a820a7d00b4377ec |
| Source note | uspto-grants-2002_04 |