Reacción #556503

ord-791f12d87530497d82841e3bc08eb5f5

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrothe grease precipitated
  2. 2
    Otrowas separated from the solvent
  3. 3
    Otroby decanting
  4. 4
    workup.DISSOLUTIONThe residue was dissolved in EtOAc
  5. 5
    Otroevaporated down
  6. 6
    Otroa little MeOH was triturated
  7. 7
    OtroThe precipitate formed
  8. 8
    Filtraciónfiltered
  9. 9
    Lavadowashed with diethyl ether
  10. 10
    Otrodried i

Procedimiento

2.08 g (9.48 mmol) 3-bromo-benzoic acid chloride, 1.41 g (9.48 mmol) 4-methyl-3H-benzoxazol-2-one and 5.33 g (40.0 mmol) aluminium trichloride were heated to 125° C. with stirring for 1.5 h. Then the mixture was mixed with ice water and the grease precipitated was separated from the solvent by decanting. The residue was dissolved in EtOAc, evaporated down and a little MeOH was triturated. The precipitate formed was suction filtered, washed with diethyl ether and dried i. vac.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08629137B2uspto-grants-2014_01