HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-(3-(Trifluoromethyl)phenyl)piperazine → HCID 22602787, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-(3-(Trifluoromethyl)phenyl)piperazine | HCID 4296 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 6-Chloronicotinamide | HCID 80456 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22602787 | HCID 22602787 | 9.1% |
Reaction Conditions
| Temperature | 120 °C |
|---|
Reaction Steps
A mixture of 6-chloro-3-pyridinecarboxamide (0.11 mol), 1-[3-(trifluoromethyl)-phenyl]-piperazine (0.1 mol) and sodium carbonate (0.22 mol) in DMF (300 ml) was stirred at 120° C. overnight. The mixture was poured out into ice water (600ml) and stirred for 1 hour. The precipitate was filtered off and dried Part of this fraction (4 g) was taken up in DCM and an aqueous NaHCO3 solution. The mixture was separated into its layers. The aqueous layer was extracted three times with DCM. The combined organic layer was dried, filtered and the solvent was evaporated till a small volume. The precipitate was filtered off and dried, yielding 3.2 g of 6-[4-[3-(trifluoromethyl)phenyl]-1-piperazinyl]-3-pyridinecarboxamide (intermediate 3).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06833369B2 |
| Source dataset | uspto-grants-2004_12 |
| ORD ID | ord-9a2611f73e3e4024ac6b6000c14e98ea |
| Source note | uspto-grants-2004_12 |