HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → 1-Phenyl-5-(trifluoromethyl)-1H-pyrazol-3-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,3-Dichloro-5,6-dicyano-1,4-benzoquinone | HCID 6775 | — |
| Reactant | 1-phenyl-5-(trifluoromethyl)-4,5-dihydro-1H-pyrazol-3-amine | HCID 67159301 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-Phenyl-5-(trifluoromethyl)-1H-pyrazol-3-amine | HCID 53403378 | 46% |
Reaction Steps
A mixture of 1-phenyl-5-(trifluoromethyl)-4,5-dihydro-1H-pyrazol-3-amine (1.47 g, 6.41 mmol) and DDQ (1.748 g, 7.7 mmol) in CH2Cl2 (30 mL) was stirred at room temperature for 4 hours. The crude product was purified by silica gel chromatography twice (with 15-35% and 10-30% EtOAc/hexane as eluants) to afford 1-phenyl-5-(trifluoromethyl)-1H-pyrazol-3-amine as an oil (0.666 g, 46%). 1H NMR (300 MHz, CDCl3) δ 7.42 (m, 5H), 6.18 (s, 1H), 3.82 (br, 2H); LC-MS (ESI) m/z 228 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08969587B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-b947d25937b04343962dae9a29f1cb22 |
| Source note | uspto-grants-2015_03 |