تفاعل #54218

ord-c6f1883f7e0b45348ac92b63ddc8c655

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةis warmed at 50° to 60° C. for 3 hours
  2. 2
    غسيلThe methylene chloride layer is washed with water and saturated aqueous saline solution in order
  3. 3
    تجفيفdried over sodium sulfate
  4. 4
    أخرىevaporated under reduced pressure
  5. 5
    أخرىto remove the solvent
  6. 6
    أخرىThe residue is crystallized from ethyl acetate/ether

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04147700uspto-grants-1979_04