HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 131716677, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-[(2-Fluorophenyl)methyl]piperazine | HCID 796168 | — |
| Reactant | HCID 15101087 | HCID 15101087 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 131716677 | HCID 131716677 | 112.6% |
Reaction Steps
A mixture of 4.8 g of 4-(chloroacetyl)-7-(3-chlorophenyl)-4,5-dihydro-6-methylpyrazolo[1,5-a]pyrimidine-3-carbonitrile, 3 g of 2-fluorobenzylpiperazine and 3.4 g of triethylamine in 200 ml of tetrahydrofuran was stirred under reflux for 18 hours, then cooled and treated with 750 ml of water. The resulting oil was extracted into dichloromethane, dried filtered and concentrated to a red-orange viscous oil. This oil was dissolved in 50 ml of acetonitrile and an excess of ether and 18 ml of 3.74N ethanolic hydrochloric acid added. After standing overnight the solid was collected, washed with ethanol and ether, dried and recrystallized from ethanol, giving 4.5 g of the desired product, mp 192°-194° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05126340 |
| Source dataset | uspto-grants-1992_06 |
| ORD ID | ord-dea97649b49748938ffb0edf4b39676e |
| Source note | uspto-grants-1992_06 |