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 of 13 g of Compound 14A in 35 mL of 37% HCl was first stirred at reflux for a period of 40 hr, followed by the addition of 30 mL water and 30 mL ethyl acetate, with the pH level adjusted to 11 through addition of a suitable quantity of 35% NaOH. The obtained organic phase was then dried over anhydrous sodium sulphate, followed by evaporation under vacuum. The obtained crude product residue was then purified by flash chromatography (chloroform—methanol 7:3). By this means, 4.46 g of Compound 14B (yield 50%) was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06271234B1 |
| Source dataset | uspto-grants-2001_08 |
| ORD ID | ord-d01832000bfb4346897097acf3f0e862 |
| Source note | uspto-grants-2001_08 |