Reacción #75119

ord-0fc569756f4846f6bd4dc3333afcf253

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaheated
  2. 2
    Temperaturatill reflux
  3. 3
    workup.STIRRINGStirring
  4. 4
    Temperaturaat reflux
  5. 5
    TemperaturaThe reaction mixture is cooled
  6. 6
    Otroevaporated
  7. 7
    workup.ADDITIONWater is added to the residue
  8. 8
    ExtracciónThe product is extracted with methylbenzene
  9. 9
    OtroThe extract is dried
  10. 10
    Filtraciónfiltered
  11. 11
    Otroevaporated
  12. 12
    OtroThe solid residue is crystallized from petroleumether
  13. 13
    FiltraciónThe product is filtered off
  14. 14
    Otrodried

Procedimiento

A mixture of 100 parts of 1-chloro-2-nitro-4-(trifluoromethyl)benzene, 90 parts of 3-amino-1-propanol and 200 parts of butanol is stirred and heated till reflux. Stirring at reflux is continued overnight. The reaction mixture is cooled and evaporated. Water is added to the residue and the whole is acidified with a hydrochloric acid solution. The product is extracted with methylbenzene. The extract is dried, filtered and evaporated. The solid residue is crystallized from petroleumether. The product is filtered off and dried, yielding 141 parts (100%) of 3-{[2-nitro-4-(trifluoromethyl)phenyl]amino}-1-propanol.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04175129uspto-grants-1979_11