HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → 2-Chloro-1-(4-(3-chlorophenyl)piperazin-1-yl)ethan-1-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Chloroacetic Acid | HCID 300 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-(3-Chlorophenyl)piperazine monohydrochloride | HCID 25681 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-Chloro-1-(4-(3-chlorophenyl)piperazin-1-yl)ethan-1-one | HCID 4165380 | 70.4% |
Reaction Steps
To solution of 1-(3-chlorophenyl)piperazine hydrochloride (1.2 g, 5.2 mmol) in DCM (10 mL) was added triethylamine (1.0 mL, 7.3 mmol), EDC (1.9 g, 10 mmol), DMAP (cat.) and chloroacetic acid (0.4 g, 5.2 mmol). The reaction was stirred at RT overnight and DCM was removed. The resultant residue was partitioned between EtOAc (50 mL) and H2O (50 mL). The organic layer was dried over Na2SO4 and concentrated to provide 1.0 g of pure 2-chloro-1-(4-(3-chlorophenyl)piperazin-1-yl)ethanone, (yield: 70%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08133998B2 |
| Source dataset | uspto-grants-2012_03 |
| ORD ID | ord-5236cf788a6a4438a99a34d8d9d28dab |
| Source note | uspto-grants-2012_03 |