HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 1-Methyl-4-[4-nitro-3-(propan-2-yloxy)phenyl]piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | 4-Fluoro-2-isopropoxy-1-nitrobenzene | HCID 10631832 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Water | HCID 962 | — |
| Product | 1-Methyl-4-[4-nitro-3-(propan-2-yloxy)phenyl]piperazine | HCID 86697983 | 97% |
Reaction Steps
A mixture of 10.0 g of 4-fluoro-1-nitro-2-(propan-2-yloxy)benzene, 10.0 g of 1-methylpiperazine and 10.4 g of potassium carbonate in 93 ml of DMSO is stirred at ambient temperature overnight. The mixture is diluted with 160 ml of water and extracted three times with 150 ml of ethyl acetate. The organic phases are dried over magnesium sulfate and concentrated under vacuum. The residue is purified on 200 g of silica, elution being carried out with dichloromethane/methanol (98/2 then 95/5), so as to obtain 13.6 g of 1-methyl-4-[4-nitro-3-(propan-2-yloxy)phenyl]piperazine in the form of a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115140B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-1b1f6372aca04743aa148a4577efee38 |
| Source note | uspto-grants-2015_08 |