HuagongsheHuagongshe Chemistry Print Report · For research reference only
Piperazine → HCID 178450871, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | HCID 178450870 | HCID 178450870 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 178450871 | HCID 178450871 | 77% |
Reaction Steps
t-Butyl 6-fluoro-1H-pyrazolo[3,4-b]pyridine-3-carboxylate (3.00 g, 0.0126 mole) was dissolved in 100 mL of toluene containing 10.85 g of piperazine (0.126 mole) and refluxed overnight. The resultant precipitate was filtered off and distributed between an aqueous NaHCO3 solution and EtOAc and then the organic phase was dried and concentrated to give a product which was recrystallized from CH3CN to give 1.57 g, mp 190°-191° C. The toluene filtrate was washed with NaHCO3 solution and then concentrated and purified by flash chromatography (EtOAc:MeOH:Et3N/16:2:2) to give an additional 1.38 g of product (total yield 77%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05300498 |
| Source dataset | uspto-grants-1994_04 |
| ORD ID | ord-c48339593c8d4211938b4992c055f936 |
| Source note | uspto-grants-1994_04 |