HuagongsheHuagongshe Chemistry Print Report · For research reference only
Piperazine → 1-(2,6-Difluoro-4-nitrophenyl)piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | 1,2,3-Trifluoro-5-nitrobenzene | HCID 2782793 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 1-(2,6-Difluoro-4-nitrophenyl)piperazine | HCID 67413372 | 96.4% |
Reaction Steps
A solution of piperazine (24 g, 0.28 mol) and 3,4,5-trifluoronitrobenzene (13 mL, 0.11 mol) in acetonitrile (200 mL) was stirred at 60° C. The progress of reaction was monitored by TLC. On completion, acetonitrile was evaporated under reduced pressure. The residue was dissolved in ethyl acetate (300 mL) and resulting solution was washed with water (100 mL), brine (100 mL), dried over anhydrous sodium sulphate and concentrated in vacuo. The residue was purified by column chromatography (silica gel, 1:9 methanol:chloroform) to provide title compound (25.8 g, 92%) as orange solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08841306B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-a9d4a88fdc2640788d0e6650632f5109 |
| Source note | uspto-grants-2014_09 |