HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 15101030, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Benzyl piperazine-1-carboxylate | HCID 643495 | — |
| Reactant | HCID 15100972 | HCID 15100972 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 15101030 | HCID 15101030 | 48.6% |
Reaction Steps
A mixture of 6.3 g of 4-(chloroacetyl)-4,5-dihydro-7-[3-(trifluoromethyl)phenyl]pyrazolo[1,5-a]pyrimidine-3-carbonitrile, 4.2 g of 1-piperazinecarboxylic acid, phenylmethyl ester and 4.1 g of triethylamine in 250 ml of tetrahydrofuran was stirred under reflux for 18 hours, then cooled and filtered. The filtrate was evaporated, the residue taken up in chloroform, washed with water, dried, filtered and concentrated. The residual oil was triturated three times with ether:hexane (1:1), then with hexane. The solid was collected, washed with hexane and dried. The solid was heated to solution in 25 ml of ethyl acetate, filtered, diluted with 25 ml of hexane and cooled, giving 4.6 g of the desired product, mp 113°-115° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05126340 |
| Source dataset | uspto-grants-1992_06 |
| ORD ID | ord-146f18f5e16c4ab9a059af2d5eea9027 |
| Source note | uspto-grants-1992_06 |