Reaktion #68488

ord-d3dd4402f7254cb68c5990ac016a0513

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.WAITThe mixture was left
  2. 2
    workup.STIRRINGto stir at 50° C. overnight
  3. 3
    Filtrationfiltered though a celite plug
  4. 4
    Extraktionthe resulting filtrate was extracted with toluene
  5. 5
    TrocknenOrganic extracts were dried over magnesium sulfate
  6. 6
    Filtrationfiltered
  7. 7
    Einengenthen concentrated

Vorschrift

To a solution of nitroethane (0.0952 ml, 1.33 mmol) in benzene (2 mL) was added phenyl isocyanate (0.291 ml, 2.66 mmol). The solution was stirred at 50° C. for ten minutes followed by the addition of triethylamine (0.00925 ml, 0.0666 mmol) and tributyl(ethynyl)stannane (0.365 ml, 1.27 mmol). The mixture was left to stir at 50° C. overnight. The solution was diluted with water and filtered though a celite plug, the resulting filtrate was extracted with toluene. Organic extracts were dried over magnesium sulfate and filtered then concentrated to yield the product as a yellow oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524900B2uspto-grants-2013_09