Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | (Chloromethyl)sulfonyl chloride | HCID 77054 | — |
| Reactant | HCID 23447422 | HCID 23447422 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 23447429 | HCID 23447429 | 81.5% |
Reaction Steps
To a solution of 1-(4-cyanobenzyl)-2-piperazinone hydrochloride (3.78 g) and triethylamine (6.27 ml) in dichloromethane (50 ml) was added a solution of chloromethanesulfonyl chloride (2.68 g) in dichloromethane (10 ml) at 0° C. and the mixture was stirred at 0° C. for 1 hour. The reaction solution was diluted with dichloromethane, washed with sodium bicarbonate solution and saturated brine, dried (MgSO4) and concentrated, and the residue was purified with silica gel column chromatography (hexane:ethyl acetate=1:2) to give colorless crystals of 4-chloromethylsulfonyl-1-(4-cyanobenzyl)-2-piperazinone (4.01 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06680312B2 |
|---|
| Source dataset | uspto-grants-2004_01 |
|---|
| ORD ID | ord-12ad702c25914681b16c3e301336d44e |
|---|
| Source note | uspto-grants-2004_01 |
|---|