Reaktion #214615

ord-54a9003f37024b16a14b58440727f723

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeprovided with an agitator
  2. 2
    TemperaturThe mixture was heated
  3. 3
    Temperaturunder reflux
  4. 4
    Sonstigethe excess thionyl chloride was removed under vacuum
  5. 5
    workup.DISSOLUTIONThe residue was dissolved in 100 ml of isopropyl ether
  6. 6
    Sonstigethe solvent removed
  7. 7
    Sonstigethe produced air-dried

Vorschrift

96 g of 6,7-dibromo-8-nitro-1,4-benzodioxane-5-carboxylic acid and 200 ml of thionyl chloride were introduced into a balloon flask provided with an agitator and a thermometer. The mixture was heated under reflux and then the excess thionyl chloride was removed under vacuum. The residue was dissolved in 100 ml of isopropyl ether and then the solvent removed and the produced air-dried. 91 g of 6,7-dibromo-8-nitro-1,4-benzodioxane-5-carbonyl chloride were obtained (M.P.: 215° C.; yield: 91%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04255580uspto-grants-1981_03