Reaktion #814023

ord-ba985a8a15ca421ab9dee434a34c716e

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture is subsequently refluxed
  2. 2
    Sonstigeto remove the gases phosgene and hydrogen chloride
  3. 3
    workup.DISTILLATIONThe batch is worked up by distillation

Vorschrift

Chlorobenzene (30 ml) is introduced into the reaction vessel at 60° C. and saturated with phosgene. A solution of 4-bromo-2-fluorobenzylamine (20.4 g, 0.10 mol) in chlorobenzene (40 ml) is added dropwise at 60° C. over 3 hours. At the same time, phosgene is passed in. Stirring of the batch is continued for 2 hours at 60° C., and the mixture is subsequently refluxed to remove the gases phosgene and hydrogen chloride. The batch is worked up by distillation. 15.9 g of 4-bromo-2-fluorobenzyl isocyanate (boiling point 109° C. at 4 mbar) are obtained. Yield: 69.1% of theory.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05710319uspto-grants-1998_01