HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → Ethyl Piperazine-2-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Diphenylpropionic acid | HCID 64798 | — |
| Reactant | 4-Benzhydryl-piperazine-2-carboxylic acid ethyl ester | HCID 14230269 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Ethyl Piperazine-2-carboxylate | HCID 10633257 | 73% |
Reaction Steps
To a solution of 4-Benzhydryl-piperazine-2-carboxylic acid ethyl ester (0.5 g, 1.54 mmol) in dry CH2Cl2 (25 ml) was added 3,3-diphenylpropanoic acid (0.35 g, 1.54 mmol) under nitrogen. To the reaction was added EDC (0.59 g, 3.08 mmol) and DMAP (cat) and the reaction mixture stirred under nitrogen at room temperature overnight. The reaction was then concentrated under reduced pressure. The residue dissolved in ethyl acetate: water (10:1) (100 ml). The organic was washed with water (20 ml, 2×) and 10% NaOH (20 ml) and dried over MgSO4 and evaporated to dryness. The resulting residue was purified by column chromatography using hexane: ethyl acetate (3:1) to give title compound in 73% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06949554B2 |
| Source dataset | uspto-grants-2005_09 |
| ORD ID | ord-c58f5ac3ecb443d783524c961cd55c6b |
| Source note | uspto-grants-2005_09 |