Reacción #54218

ord-c6f1883f7e0b45348ac92b63ddc8c655

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturais warmed at 50° to 60° C. for 3 hours
  2. 2
    LavadoThe methylene chloride layer is washed with water and saturated aqueous saline solution in order
  3. 3
    Secadodried over sodium sulfate
  4. 4
    Otroevaporated under reduced pressure
  5. 5
    Otroto remove the solvent
  6. 6
    OtroThe residue is crystallized from ethyl acetate/ether

Procedimiento

A suspension of 5-chloro-2-[3-(2-chloroacetamidomethyl)-5-methyl-4H-1,2,4-triazol-4-yl]-benzophenone (1.35g) and potassium phthalimide (0.7 g) in dimethylformamide (10 ml) is warmed at 50° to 60° C. for 3 hours. The reaction mixture is shaken with methylene chloride. The methylene chloride layer is washed with water and saturated aqueous saline solution in order, dried over sodium sulfate and evaporated under reduced pressure to remove the solvent. The residue is crystallized from ethyl acetate/ether to give 5-chloro-2-[3-(2-phthalimido-acetamidomethyl)-5-methyl-4H-1,2,4-triazol-4-yl]-benzophenone as crystals melting at 251° to 253° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04147700uspto-grants-1979_04