HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 21830779, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1-(3-(Trifluoromethyl)phenyl)piperazine | HCID 4296 | — |
| Reactant | O-Xylene | HCID 7237 | — |
| Reactant | 2-(4-Chloro-butyl)-2H-[1,2,4]triazine-3,5-dione | HCID 15817175 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 21830779 | HCID 21830779 | 26.3% |
Reaction Steps
The compound 1b (6.67 g; 0.033 mol) and 4-(3-trifluoromethylphenyl)piperazine (15.3 g; 0.066 mol) are heated to dryness for 7 hours at 120-130° C. Xylene (40 ml) is added and heated for one additional hour under reflux. After cooling and concentrating to dryness under vacuum, the residue is taken up in water (30 ml) and in ethyl ether (2×100 ml). The organic phases are dried (Na2SO4) and concentrated to dryness under vacuum. The oil obtained is taken up in ethyl ether (50 ml) and then supplemented, dropwise, with hydrochloric acid in ethyl ether (20 ml). A solid is drained which is crystallized from ethanol (50 ml). After filtration, washing with ethyl ether and drying under vacuum at 80° C., the compound 1 (3.77 g) is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05977106 |
| Source dataset | uspto-grants-1999_11 |
| ORD ID | ord-8405128157ea44808a286e2bfb87b351 |
| Source note | uspto-grants-1999_11 |