Reaktion #814024

ord-f9950dc95a94410486aae253107a9552

Lösungsmittel

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

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

Vorschrift

A solution of 4-bromo-2-fluorobenzylamine (20.4 g, 0.10 mol) in toluene (300 ml) is saturated with gaseous hydrochloric acid at 25° C. The resulting suspension of the 4-bromo-2-fluorobenzylamine hydrochloride is heated at 100° C. Phosgene is passed in at this temperature. Stirring of the solution, which has eventually become clear, is continued at 100° C. for 1 hour, and the mixture is then refluxed to remove the gases phosgene and hydrogen chloride. The batch is worked up by distillation. 21.2 g of 4-bromo-2-fluorobenzyl isocyanate (boiling point 109° C. at 4 mbar) are obtained. Yield: 92.1% of theory.

Quelle

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