Reaktion #476860
ord-9d5ab9fcdb5542cba0f96af3891d264f
Reaktionsgleichung
Edukte
Reagenzien
Lösungsmittel
Reaktionsbedingungen
Temperatur
110°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturAfter cooling to RT the reaction mixture
- 2Sonstigewas quenched by the addition of 100 ml water
- 3Extraktionextracted with ethyl acetate (three times)
- 4Waschenwashed with water and sat. aq NaCl-solution
- 5Trocknendried with Na2SO4
- 6Filtrationfiltered
- 7Sonstigeevaporated to dryness
- 8Sonstigepurified by silica gel chromatography
Vorschrift
Intermediate 83 (7 g, 23.87 mmol), pyrrolidin-2-one (4.06 g, 47.74 mmol), CuI (909 mg, 4.77 mmol), N,N′-dimethylethylene diamine (10.28 ml, 95.49 mmol) and K2CO3 (7.25 g, 52.52 mmol) were suspended in toluene (10 ml) under N2 and heated to 110° C. for 16 h. After cooling to RT the reaction mixture was quenched by the addition of 100 ml water and extracted with ethyl acetate (three times). The organic layers were combined and washed with water and sat. aq NaCl-solution, dried with Na2SO4, filtered and evaporated to dryness, and purified by silica gel chromatography.