HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylenediamine → HCID 15329237, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylenediamine | HCID 3301 | — |
| Reactant | 3-(4-Chlorobenzoyl)propionic acid | HCID 77604 | — |
| Catalyst | Hydrochloric Acid | HCID 313 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 15329237 | HCID 15329237 | 81.4% |
Reaction Steps
To a solution of 3-(4-chlorobenzoyl)propionic acid (40 g, 190 mmol) in xylene (250 mL) were added ethylenediamine (22.6 g, 376 mol), and 12M hydrochloric acid (0.500 mL, 6 mmol). The reaction mixture was stirred at reflux under Dean-Stark for 12 h, and cooled to RT. The solid was collected by filtration and washed with xylene to give the crude residue. This was dissolved in DCM (400 ml) and filtered. The filtrate was concentrated in vacuo to give 36.6 g (62%) of the racemic title compound as a beige solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08592403B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-35e252ac95604548b63c8d2d8704483e |
| Source note | uspto-grants-2013_11 |