HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → HCID 15100973, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | HCID 15100972 | HCID 15100972 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 15100973 | HCID 15100973 | 34.9% |
Reaction Steps
A mixture of 1.3 g of N-methylpiperazine, 4.4 g of 4-(chloroacetyl)-4,5-dihydro-7-[3-(trifluoromethyl)phenyl]pyrazolo[1,5-a]pyrimidine-3-carbonitrile and 1.5 g of sodium carbonate in 75 ml of toluene was refluxed for 4 hours, then allowed to stand at room temperature overnight. The mixture was treated with 30 ml of 1N sodium hydroxide and the phases were separated. The aqueous phase was extracted twice with chloroform. The organic phases were combined, washed with water, dried, filtered and concentrated. The residue was heated to solution in 50 ml of ethyl acetate, filtered and cooled. The crystalline solid was collected, washed with ethyl acetate and hexane and dried, giving 1.8 g of the desired product, mp 178°-180° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05219857 |
| Source dataset | uspto-grants-1993_06 |
| ORD ID | ord-f1553489a2e047d3a7bc1b378a184290 |
| Source note | uspto-grants-1993_06 |