HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Chlorobenzenesulfonyl chloride → HCID 9846568, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Chlorobenzenesulfonyl chloride | HCID 7398 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 18328910 | HCID 18328910 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 9846568 | HCID 9846568 | 76.9% |
Reaction Steps
A solution of 4-chlorophenylsulphonyl chloride (1.78 g) in methylene chloride (10 ml) was added dropwise over 15 minutes to a mixture of 4-[1-(2-methylpyrimidin-4-yl)piperazine-4-ylmethyl]piperidine trihydrochloride (2.78 g) and triethylamine (6.72 ml) in dichloromethane (40 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 4% methanol in dichloromethane. Recrystallisation from ethyl acetate/hexane gave, as a solid 1-(4-chlorophenylsulphonyl)-4-[1-(2-methylpyrimidin-4-yl)piperazin-4ylmethyl]piperidine (2.50 g), mp 191-193° C. (decomp.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06335341B1 |
| Source dataset | uspto-grants-2002_01 |
| ORD ID | ord-0b85241f0333445599018e83613de919 |
| Source note | uspto-grants-2002_01 |