Reacción #981807

ord-e6844d638f9a4e05aa72564fcbfd7946

Condiciones de reacción

Temperatura
-17°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Extracciónextracted with ethyl acetate
  2. 2
    LavadoThe extract was washed with water
  3. 3
    Otrodried
  4. 4
    OtroThe solvent was evaporated off
  5. 5
    Otrothe residue was recrystallized from ethanol-water

Procedimiento

5-Aminospiro[benzo[b]furan-2(3H),1'-cyclopropane]-3-one (0.747 g.) and calcium carbonate (0.47 g.) were suspended in a mixture of carbon tetrachloride (20 ml.) and methylene chloride (5 ml.). The suspension was cooled to -17° C., then bromine (0.22 ml.) was added thereto dropwise, followed by stirring for 45 minutes. The reaction mixture was poured into ice-water, then extracted with ethyl acetate. The extract was washed with water and dried. The solvent was evaporated off, and the residue was recrystallized from ethanol-water. By the above procedure there was obtained 5-amino-4-bromospiro[benzo[b]furan-2(3H),1'-cyclopropane]-3-one as yellow needles melting at 167°-170° C. Yield 0.6 g.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04284644uspto-grants-1981_08