HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 5-Amino-3-tert-butyl-1-(2-methylpyridine-5-yl)pyrazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Pentanenitrile, 4,4-dimethyl-3-oxo- | HCID 108871 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 5-Hydrazinyl-2-methylpyridine | HCID 22147137 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 5-Amino-3-tert-butyl-1-(2-methylpyridine-5-yl)pyrazole | HCID 11401974 | 62% |
Reaction Steps
A solution of 5-hydrazino-2-methyl-pyridine (8.0 g, 65.0 mmol) and 4,4-dimethyl-3-oxopentanenitrile (10.0 g, 79.9 mmol) in EtOH (200 mL) containing 6 N HCl (6 mL) was refluxed for 17 h, then cooled to room temperature. Solid sodium hydrogen carbonate was added to neutralize the solution. The slurry was filtered. The filtrate was concentrated. Column chromatography (silica gel, 2.5″×5″, eluant=EtOAc) afforded the desired 5-amino-3-tert-butyl-1-(2-methylpyridine-5-yl)pyrazole (9.21 g, 62%) as a tan solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06525046B1 |
| Source dataset | uspto-grants-2003_02 |
| ORD ID | ord-41f3fe7cc7d549d1b1936b42f9957505 |
| Source note | uspto-grants-2003_02 |