HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 19791265, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1-[2-[Bis(4-fluorophenyl)methoxy]ethyl]piperazine | HCID 9974013 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | HCID 19791265 | HCID 19791265 | 82.8% |
Reaction Steps
To a solution of 1-[2-[bis(4-fluorophenyl)-methoxy]ethyl]piperazine (1 g) in 1N-hydrochloric acid (3 ml) was added 1N-hydrochloric acid in order to adjust pH to 4. The mixture was stirred at 70°-75° C. and therein a solution of sodium nitrite (0.31 g) in water (0.5 ml) was added dropwise. The mixture was stirred at 70°-75° C. for one hour, cooled, and diluted with a mixture of diethyl ether and aqueous sodium bicarbonate solution. The organic layer was washed withbrine, dried, and concentrated in vacuo. The residue was purified by column chromatography on silica gel eluted with chloroform to yield 1-[2-[bis(4-fluorophenyl)methoxy]ethyl]-4-nitrosopiperazine (0.9 g) as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05250528 |
| Source dataset | uspto-grants-1993_10 |
| ORD ID | ord-5e18d197f10542e69a85662a383fbcb3 |
| Source note | uspto-grants-1993_10 |