HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Methylpiperazine → 1-(4-Methoxy-3-nitrophenyl)-4-methylpiperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | 4-Bromo-2-nitroanisole | HCID 118533 | — |
| Reactant | 2-(Dicyclohexylphosphino)-2'-(dimethylamino)biphenyl | HCID 2734217 | — |
| Catalyst | palladium(II) acetate | HCID 167845 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1-(4-Methoxy-3-nitrophenyl)-4-methylpiperazine | HCID 59441886 | 55% |
Reaction Steps
Pd(OAc)2 (85 mg, 0.38 mmol), 2-dicyclohexylphosphino-2′-(N,N-dimethylamino)-biphenyl (225 mg, 0.57 mmol), K3PO4 (2.26 g, 10.68 mmol), 4-bromo-1-methoxy-2-nitro-benzene (1.77 g, 7.63 mmol) in THF (50 mL) were charged in a round-bottom flask flushed with argon. The flask was evacuated and backfilled with argon. N-methylpiperazine (1.01 mL, 9.15 mmol) was added and the reaction mixture was refluxed for 72 h. The reaction mixture was then allowed to cool to room temperature and concentrated. The crude solid was purified by flash chromatography on silica gel (eluant: DCM/EtOH 90/10) to afford 1.05 g (55% yield) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08614220B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-be86d5097a98409bba6438de9968a2d9 |
| Source note | uspto-grants-2013_12 |