HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 1-[(2,5-Dichlorophenyl)methyl]piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Ethyl 4-(2,5-dichlorobenzyl)piperazine-1-carboxylate | HCID 22458123 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | 1-[(2,5-Dichlorophenyl)methyl]piperazine | HCID 4643368 | 50% |
Reaction Steps
A solution containing 13 g of 1-(2,5-dichlorobenzyl)-4-ethoxycarbonylpiperazine in 35 mL of 37% HCl was stirred for 40 h at reflux. Subsequently, 30 mL of water and 30 mL of EtOAc were added at room temperature, adjusting the pH to 11 via addition of 35% NaOH. The organic phase, which was dried on anhydrous sodium sulphate, was evaporated to dryness under vacuum. The crude was purified via flash chromatography (CHCl3-MeOH 7:3) giving 4.46 g (50%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06399614B1 |
| Source dataset | uspto-grants-2002_06 |
| ORD ID | ord-1dd7c67e968a4bd5929469251247f67a |
| Source note | uspto-grants-2002_06 |