HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Bromobenzenesulfonyl chloride → 1-(4-Bromophenylsulphonyl)-4-[1-(3-fluoro-4-pyridyl)piperidin-4-ylcarbonyl]piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Bromobenzenesulfonyl chloride | HCID 7396 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 18432756 | HCID 18432756 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-(4-Bromophenylsulphonyl)-4-[1-(3-fluoro-4-pyridyl)piperidin-4-ylcarbonyl]piperazine | HCID 18432758 | 65.3% |
Reaction Steps
4-Bromophenylsulphonyl chloride (1.02 g) was added to a mixture of 1-[1-(3-fluoro-4-pyridyl)-piperidin-4-ylcarbonyl]piperazine hydrochloride (1.22 g) and triethylamine (3.70 ml) in dichloromethane (45 ml) at 0° C. The solution was stirred at ambient temperature for 18 hours. The solution was diluted with dichloromethane and washed with water, dried (Na2SO4) and evaporated. The residue was purified by chromatography eluting with 2% methanol in dichloromethane. Recrystallisation from ethyl acetate/hexane gave 1-(4-bromophenylsulphonyl)-4-[1-(3-fluoro-4-pyridyl)piperidin-4-ylcarbonyl]piperazine (1.24 g) as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06440972B1 |
| Source dataset | uspto-grants-2002_08 |
| ORD ID | ord-e706fc2caf814903b79f60f484f548b6 |
| Source note | uspto-grants-2002_08 |