Reacción #76156

ord-a5737dce6e764e158f8936e8ce98673c

Reactivos

Ninguno

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaThe mixture was refluxed
  2. 2
    TemperaturaIt was cooled
  3. 3
    Otrothe trifluoroacetic acid was removed under reduced pressure
  4. 4
    workup.ADDITIONThe solution was mixed with 150 mL water
  5. 5
    Filtraciónthe resulting precipitate was filtered
  6. 6
    Lavadowashed with hexane
  7. 7
    Otrodried

Procedimiento

Ethyl 2,6-dichloro-5-fluoronicotinate (1) (30.0 g) was dissolved in a mixture of 60 mL of trifluoro acetic acid and 60 mL of 7.5 N HCl. The mixture was refluxed with stirring for 26 h. It was cooled and the trifluoroacetic acid was removed under reduced pressure. The solution was mixed with 150 mL water, the resulting precipitate was filtered, washed with hexane and dried to yield 16.5 g of 2,6-dichloro-5-fluoro nicotinic acid (2). m.p.=152-156° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06699989B1uspto-grants-2004_03