HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl chloroformate → 4-Ethoxycarbonyl-1-(2-pyrrolidone-5-carbonyl)piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-(2-Pyrrolidone-5-carbonyl)piperazine | HCID 14053693 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 4-Ethoxycarbonyl-1-(2-pyrrolidone-5-carbonyl)piperazine | HCID 14053696 | 84.3% |
Reaction Steps
A mixed solution of 2.1 g of 1-(2-pyrrolidone-5-carbonyl)piperazine, 2.5 g of anhydrous potassium carbonate and 120 ml of acetonitrile was cooled with ice water and 1.1 g of ethyl chlorocarbonate in 10 ml of acetonitrile was dropped therein with stirring. After dropping, the mixture was stirred overnight at room temperature. The solvent was evaporated from the reaction mixture in vacuo, methylene chloride was added to the residue, and insoluble matter was removed therefrom by filtration. The solvent was evaporated in vacuo from the filtrate to give 2.3 g of oily product. This was crystallized from ethyl acetate and further recrystallized to give 2.1 g of desired product, m.p. 147°-148.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05102882 |
| Source dataset | uspto-grants-1992_04 |
| ORD ID | ord-c837943f505245a6abfc60d17b48dbb2 |
| Source note | uspto-grants-1992_04 |