Reaktion #476860

ord-9d5ab9fcdb5542cba0f96af3891d264f

Lösungsmittel

Reaktionsbedingungen

Temperatur
110°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling to RT the reaction mixture
  2. 2
    Sonstigewas quenched by the addition of 100 ml water
  3. 3
    Extraktionextracted with ethyl acetate (three times)
  4. 4
    Waschenwashed with water and sat. aq NaCl-solution
  5. 5
    Trocknendried with Na2SO4
  6. 6
    Filtrationfiltered
  7. 7
    Sonstigeevaporated to dryness
  8. 8
    Sonstigepurified 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08378092B2uspto-grants-2013_02