HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → Diethyl 3-ethyl-5-oxo-2,2-pyrrolidinedicarboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Acetamidomalonic acid diethyl ester | HCID 14041 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Reactant | Ethyl trans-2-pentenoate | HCID 5367761 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | Diethyl 3-ethyl-5-oxo-2,2-pyrrolidinedicarboxylate | HCID 255944 | 87.1% |
Reaction Steps
To 150 mg of sodium dissolved in 150 mL of absolute ethanol was added diethyl acetamidomalonate (5.3 g, 25 mmol) and ethyl-(2E)-pent-2-enoate (3.5 g, 27.3 mmol). The reaction mixture was then refluxed for 20 h. After this period of time, 2 mL of glacial acetic acid was added, volatiles were removed under pressure with the aid of a water aspirator and heating bath. On cooling the residue solidified. The residue was dissolved in 50 mL of toluene and to this was added 20 mL of petroleum ether. The product precipitated when the mixture was cooled. The crystals were collected and washed with water and further dried in vacuo to obtain a white solid (5.6 g, 79.77%). Mass Spectrum (+ESI): 258 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06610734B2 |
| Source dataset | uspto-grants-2003_08 |
| ORD ID | ord-b5ab014544dc499db845b4e00332b6e7 |
| Source note | uspto-grants-2003_08 |