Reaktion #323171

ord-94979adb2c224e2eab50346924169805

Lösungsmittel

Reaktionsbedingungen

Temperatur
195°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenthe resulting solution is washed with water twice
  2. 2
    TrocknenThe dichloromethane solution is dried
  3. 3
    Sonstigeevaporated
  4. 4
    workup.DISTILLATIONthe residue distilled at reduced pressure
  5. 5
    SonstigeThe distillate is recrystallized from hot hexane

Vorschrift

A mixture of 3-chlorophenyl isocyanate (7.65 g, 50 mmoles), N-(2-chloroethyl)-2-oxazolidinone (7.5 g, 50 mmoles) and anhydrous AlCl3 (40 mg, 0.3 mmole) is heated at 195° C. for 6 hours with stirring. The reaction mixture is dissolved in dichloromethane and the resulting solution is washed with water twice. The dichloromethane solution is dried and evaporated and the residue distilled at reduced pressure. The distillate is recrystallized from hot hexane to give 10.2 g (78.4 percent) of the desired product, m.p. 64° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04642351uspto-grants-1987_02