HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 4-(2,3-Dichlorobenzoyl)piperazin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,3-Dichlorobenzoyl chloride | HCID 17944 | — |
| Reactant | Piperazin-2-one | HCID 231360 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | 4-(2,3-Dichlorobenzoyl)piperazin-2-one | HCID 31096043 | — |
Reaction Steps
To a suspension of 2-piperazinone (5.3 g, 52.9 mmol, commercially available e.g. from Sigma-Aldrich) in dry Dichloromethane (DCM) (76 ml) was added triethylamine (16.23 ml, 116 mmol) and finally 2,3-dichlorobenzoyl chloride (12.20 g, 58.2 mmol, commercially available e.g. from ABCR, ChemPacific or UkrOrgSynthesis) dropwise (exothermic). The mixture was stirred at room temperature. After 1 hour the mixture was diluted with Dichloromethane (DCM) (150 mL) and saturated NaHCO3 solution (150 ml), the phases were separated and the aqueous layer was extracted with DCM (2×100 ml). The combined organic fractions were washed with brine and dried over MgSO4. Evaporation gave 4-[(2,3-dichlorophenyl)carbonyl]-2-piperazinone (12 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08501946B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-146fdf2700e149978f369c205f940190 |
| Source note | uspto-grants-2013_08 |