반응 #54218

반응 방정식

5-chloro-2-[3-(2-chloroacetamidomethyl)-5-methyl-4H-1,2,4-triazol-4-yl]-benzophenone

potassium phthalimide

methylene chloride

→

5-chloro-2-[3-(2-phthalimido-acetamidomethyl)-5-methyl-4H-1,2,4-triazol-4-yl]-benzophenone

용매

dimethylformamide

반응 조건

후처리

1. 1
   온도is warmed at 50° to 60° C. for 3 hours
2. 2
   세척The methylene chloride layer is washed with water and saturated aqueous saline solution in order
3. 3
   건조dried over sodium sulfate
4. 4
   기타evaporated under reduced pressure
5. 5
   기타to remove the solvent
6. 6
   기타The residue is crystallized from ethyl acetate/ether

실험 절차

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.

출처