HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-methyl-1H-pyrazol-4-amine → HCID 178481770, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-methyl-1H-pyrazol-4-amine | HCID 4770990 | — |
| Reactant | HCID 21959055 | HCID 21959055 | — |
| Catalyst | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 178481770 | HCID 178481770 | 46% |
Reaction Steps
A solution of 1-methyl-1H-pyrazol-4-amine ((J. Catalan et al., J. Heterocycl. Chem., 1985, 22, 997), 200 mg, 2.06 mmol), 2-oxocyclohexanecarboxylate (351 mg, 2.06 mmol), and p-toluenesulfonic acid monohydrate (10 mg, 0.05 mmol) in toluene (20 ml) was stirred at 120° C. for 2.5 h. After cooling to room temperature, the solvent was removed in vacuo. Diphenyl ether (5 ml) was added to the residue (ca. 300 mg) and the resulting mixture was heated at 240° C. for 40 min. After cooling to room temperature, hexane (2 ml) was added. The precipitate was collected by filtration and washed with dichloromethane to give 190 mg (46%) of the title compound as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06686373B2 |
| Source dataset | uspto-grants-2004_02 |
| ORD ID | ord-2a889fbc4de945e98e283b924c1682de |
| Source note | uspto-grants-2004_02 |