HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid → HCID 59210396, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 59210383 | HCID 59210383 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 59210396 | HCID 59210396 | 55.3% |
Reaction Steps
Ethyl 4,4,4-trifluoro-2-(3-methyl-4-nitro-benzyl)-3-oxo-butyrate (2.0 g), hydrazine monohydrate (0.5 g) and a small amount of p-toluenesulfonic acid were dissolved in toluene, and the mixture was refluxed for 4 hours. After cooling, the solvent was distilled off under reduced pressure. The residue was suspended in ethyl acetate and washed with 1N aqueous solution of hydrochloric acid. After drying the organic layer with sodium sulfate, the solvent was distilled off and the obtained residue was purified by silica gel column chromatography to obtain 4-(3-methyl-4-nitro-benzyl)-5-trifluoromethyl-2,4-dihydro-pyrazol-3-one (1.0 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07674807B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-f1fb38fb7ca94ea48e82ff0bdc38bf35 |
| Source note | uspto-grants-2010_03 |