HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 178513405, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 11164124 | HCID 11164124 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178513405 | HCID 178513405 | 20.3% |
Reaction Steps
A stirred mixture of 4-trifluoromethyl-2-(4-trifluoromethyl-phenyl)-imidazo[1,5-a]pyrimidine-8-carbonitrile [CAS-No. 851263-42-8] 1.16 g, 3.26 mmol), hydroxylamine hydrochloride (0.46 g, 6.62 mmol) and potassium carbonate (1.35 g, 9.77 mmol) in ethanol (50 ml) was heated under reflux conditions for 3 h. The precipitate was collected by filtration and washed with ethanol, the combined filtrates were evaporated and the crude product purified by column chromatography on silica gel (ethyl acetate/ethanol 95:5) and crystallization from diethyl ether/hexane to yield the title compound (257 mg, 20%) as a red solid. MS (ISN) 388.2 [(M−H)−]; mp 213° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07504404B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-6975fa515ba4400b8ffc0b36dae7d9f5 |
| Source note | uspto-grants-2009_03 |