Réaction #96166

ord-f1ff1f771c8f4e70be8891939feaf0e1

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températuremaintaining the temperature of the reaction mixture below 50° C
  2. 2
    AutreThe ice bath is then removed
  3. 3
    Autreevaporated to dryness under reduced pressure
  4. 4
    workup.ADDITIONof benzene is added to the residue
  5. 5
    Autrethe solution is evaporated under vacuum once again
  6. 6
    Autreto completely remove the excess hydrogen chloride

Mode opératoire

A solution of 1.34 g. of 5-benzoyl-7-bromo-1,2-dihydro-3H-pyrrolo[1,2-a]pyrrole-1-carboxylic acid in 50 ml. of isopropanol, cooled in an ice bath is saturated with gaseous hydrogen chloride, maintaining the temperature of the reaction mixture below 50° C. The ice bath is then removed and the reaction mixture is stirred for 1.5 hours at room temperature, and evaporated to dryness under reduced pressure; 10 ml. of benzene is added to the residue and the solution is evaporated under vacuum once again, repeating this process a total of three times to completely remove the excess hydrogen chloride, thus obtaining of isopropyl 5-benzoyl-7-bromo-1,2-dihydro-3H-pyrrolo[1,2-a]pyrrole-1-carboxylate. The product is recrystallized from methanol-ethyl acetate.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US04347185uspto-grants-1982_08