HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazinium bromide → 5-methyl-4-(pyridin-3-yl)-1H-pyrazol-3-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazinium bromide | HCID 159693 | — |
| Reactant | 3-Oxo-2-(pyridin-3-yl)butanenitrile | HCID 67362649 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | 5-methyl-4-(pyridin-3-yl)-1H-pyrazol-3-amine | HCID 67363636 | — |
Reaction Steps
3-Oxo-2-pyridin-3-yl-butyronitrile (step 1) (1.00 g, 6.49 mmol) was dissolved in EtOH (10 ml) and water (2 ml). Hydrazine hydrobromide (2.82 g, 24.97 mmol) was added and the reaction mixture was heated at reflux for 1 hour. The solvent was removed in vacuo and the residue was partitioned between EtOAc and sat. NaHCO3. The organic phase was washed with water and brine, dried (MgSO4), filtered and the solvent was removed in vacuo to afford the title compound which was used without further purification; 1H NMR (d6-DMSO, 400 MHz) δ 11.51 (1H, br), 8.60 m), 8.40 (1H, m), 7.72 (1 h, m), 7.39 (1H, m), 4.60 (2H, br), 2.19 (3H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08835444B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-50f9fa1b87994be683590f893a48119e |
| Source note | uspto-grants-2014_09 |