HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → (S)-1-(3-hydroxypropyl)-2-(N,N-dimethylcarbamoyl)pyrrolidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 3-Bromo-1-propanol | HCID 12308 | — |
| Reactant | (2S)-N,N-dimethylpyrrolidine-2-carboxamide | HCID 7408249 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | (S)-1-(3-hydroxypropyl)-2-(N,N-dimethylcarbamoyl)pyrrolidine | HCID 54383891 | 48.3% |
Reaction Steps
A mixture of (S)-2-(N,N-dimethylcarbamoyl)pyrrolidine (426 mg, 3 mmol), (Chem. pharm. Bull. 1973, 21, 2112-2116), 3-bromo-1-propanol (0.41 ml, 4.5 mmol) and potassium carbonate (829 mg, 6 mmol) in acetonitrile (6 ml) was heated at reflux for 8 hours. The mixture was allowed to cool and was partitioned between methylene chloride and water. The organic layer was separated, washed with brine, dried (MgSO4) and the solvent removed by evaporation. The residue was purified by column chromatography, eluting with methylene chloride/methanol (a gradient from 90/10 to 60/40) to give (S)-1-(3-hydroxypropyl)-2-(N,N-dimethylcarbamoyl)pyrrolidine (290 mg, 48%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | USRE042353E1 |
| Source dataset | uspto-grants-2011_05 |
| ORD ID | ord-e9101b04e98e44efacaeb2d72ddc3fc7 |
| Source note | uspto-grants-2011_05 |