HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Pyrrolidone → 1-Phenoxycarbonyl-2-oxopyrrolidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Pyrrolidone | HCID 12025 | — |
| Reactant | Phenyl chloroformate | HCID 15891 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1-Phenoxycarbonyl-2-oxopyrrolidine | HCID 14441090 | 100.1% |
Reaction Conditions
| Temperature | -60 °C |
|---|
Reaction Steps
To a solution of 7.36 g (184 mmol) of NaH (60%) in 200 ml of THF was added 15.68 g (184 mmol) of 2-oxopyrrolidine with stirring under ice-cooling, and further the mixture was stirred at room temperature for 1 hr. until H2 gas ceased to evolve. The reaction solution was added to a solution of 29.7 g (190 mmol) of phenyl chloroformate in 100 ml of THF cooled at -60° C. and then stirred at room temperature for 4 hr. The reaction solution was poured into ice water, and then extracted with ethyl acetate. After drying, the solvent was removed by evaporation. When the crystalline residue was recrystallized from CH2CL2 - ether, 37.8 g of the objective compound (II) melting at 120.0°-121.5° C. was obtained as crystals. Yield:84.0%
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05202345 |
| Source dataset | uspto-grants-1993_04 |
| ORD ID | ord-f5decf36365541e09b26d65cd800bc71 |
| Source note | uspto-grants-1993_04 |