HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-(Trimethylsilyl)pyrrolidin-2-one → HCID 67883823, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-(Trimethylsilyl)pyrrolidin-2-one | HCID 84461 | — |
| Reactant | Tetrabutylammonium Fluoride Trihydrate | HCID 11726816 | — |
| Reactant | HCID 13149080 | HCID 13149080 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67883823 | HCID 67883823 | — |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
3.24 g (20 mmol) of 4,5-epoxy-2,3,4,5-tetrahydro-1-benzoxepin and 9.60 g (61 mmol) of N-trimethylsilyl-2-oxo-pyrrolidine are dissolved in 8 ml of dry THF and, while cooling, 6.31 g (20 mmol) of tetrabutylammonium fluoride trihydrate are added in one portion, and the mixture is heated at 100° C. for several hours (TLC check). The mixture is hydrolyzed with ice-water and extracted several times with diethyl ether. The combined diethyl ether extracts are washed with saturated sodium chloride solution and dried over sodium sulfate. After filtration and evaporation of the solvent in vacuo, the residue is crystallized in diisopropyl ether/ethyl acetate. Crystals of melting point 151°-153° C. are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05194442 |
| Source dataset | uspto-grants-1993_03 |
| ORD ID | ord-9fa850d5e3aa4b0090d554099ca5bc25 |
| Source note | uspto-grants-1993_03 |