HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 178513391, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | 5-(4-Trifluoromethyl-phenyl)-7-trifluoromethyl-pyrazolo[1,5-a]pyrimidine-3-carbonitrile | HCID 11405592 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178513391 | HCID 178513391 | 69.1% |
Reaction Steps
A stirred mixture of 7-trifluoromethyl-5-(4-trifluoromethyl-phenyl)-pyrazolo[1,5-a]pyrimidine-3-carbonitrile [CAS-No. 851262-50-5] (2.0 g, 5.61 mmol), hydroxylamine hydrochloride (0.78 g, 11.2 mmol) and potassium carbonate (2.33 g, 16.8 mmol) in ethanol (100 ml) was heated under reflux conditions for 3 h. After the reaction mixture reached room temperature the precipitate was collected by filtration and washed with ethanol and ethyl acetate. The combined filtrates were evaporated and the crude product purified by flash chromatography on silica gel (ethyl acetate/heptane) to yield the title compound (1.51 g, 69%) as an orange solid. MS (ISP) 389.9 [(M+H)+]; mp 252° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08093263B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-9d49e94b8ada4b98886d3d0b7f523268 |
| Source note | uspto-grants-2012_01 |