HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 17798577, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | m-Bromobenzenesulphonyl chloride | HCID 17943 | — |
| Reactant | HCID 10858694 | HCID 10858694 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 17798577 | HCID 17798577 | 26% |
Reaction Steps
To a solution of 1-[1-(4-pyridyl)-4-piperidylmethyl]-2-piperazinone (2.74 g) and triethylamine (1.67 ml) in dichioromethane (50 ml) was added dropwise at 0° C. 3-bromobenzenesulfonyl chloride (2.56 g), and the mixture was stirred at 0° C. for 1 hour. The reaction solution was diluted with dichioromethane, was washed with water and saturated brine, dried (MgSO4) and concentrated, and the residue was purified with silica gel column chromatography (acetone methanol=9:1=>1:1) and washed with water to give colorless crystals of 4-(3-bromobenzenesulfonyl)-1-[1-(4-pyridyl)-4-piperidylmethyl]-2-piperazinone (1.28 g). A part of the crystals were treated with hydrochloric acid to give colorless crystals of the title compound as hydrochloride.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06680312B2 |
| Source dataset | uspto-grants-2004_01 |
| ORD ID | ord-f8d7618cf9674fd49c994ed566fc6237 |
| Source note | uspto-grants-2004_01 |