HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 3-Chloro-1-phenylpyrrolidin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| Reactant | 1-Phenylpyrrolidin-2-one | HCID 78375 | — |
| Reactant | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 3-Chloro-1-phenylpyrrolidin-2-one | HCID 21935559 | — |
Reaction Steps
1-Phenyl-2-pyrrolidinone (1 g, 6.2 mmol) in THF (60 mL, anhydrous) was cooled to −40° C. and LiHMDS (8 mL, 8 mmol, 1 M soln. in THF) was added. The resulting solution was stirred for 40 min. and tosyl chloride (1.78 g, 9.33 mmol) was then added. After warming the solution to RT over a 14 hour period, H2O added to quench reaction. The solution was then concentrated to provide an oil. Next, the oil was redissovled in EtOAc and washed with H2O and brine. The organic layer was dried over Na2SO4, filtered, and concentrated to an oil once again. Purified via flash column chromatography (4:1 hexane/EtOAc) provided 3-chloro-1-phenylpyrrolidin-2-one.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07262198B2 |
| Source dataset | uspto-grants-2007_08 |
| ORD ID | ord-9b6bd28499c3486b8c1be729557a3056 |
| Source note | uspto-grants-2007_08 |