HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → Tert-butyl 4-(methylsulfonyl)piperazine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Tert-butyl 4-(methylsulfonyl)piperazine-1-carboxylate | HCID 4496004 | — |
Reaction Steps
In dichloromethane (40 ml), N-tert-butoxycarbonylpiperazine (2.00 g) was dissolved, followed by the addition of triethylamine (1.78 ml). To the resulting solution, methanesulfonyl chloride (0.91 ml) was added dropwise under ice cooling. After stirring for one hour under ice cooling, the reaction mixture was diluted with dichloromethane (20 ml), washed with a 5% aqueous citric acid solution, water and saturated saline and dried over anhydrous magnesium sulfate. The residue obtained by distilling off the solvent under reduced pressure was recrystallized from a mixed solvent of ethyl acetate and hexane, whereby the title compound (2.58 g, 91%) was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06525042B1 |
| Source dataset | uspto-grants-2003_02 |
| ORD ID | ord-f4b64ab5f6f044caa059caba390f4524 |
| Source note | uspto-grants-2003_02 |