Reaktion #54215

Reaktionsgleichung

ethyl acetate

sodium bicarbonate

2-phthalimidoacetyl chloride

5-chloro-2-(3-aminomethyl-5-methyl-4H-1,2,4-triazol-4-yl)-benzophenone dihydrobromide

→

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

Ausbeute 69.4%

Lösungsmittel

benzene

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeis gradually returned to room temperature
2. 2
   Sonstigeto stand at room temperature
3. 3
   FiltrationThe precipitated crystals are filtered
4. 4
   Waschenwashed with methanol
5. 5
   Sonstigedried

Vorschrift

To a solution of 2-phthalimidoacetyl chloride (1.5 g) in benzene (20 ml) and dimethylformamide (10 ml), 5-chloro-2-(3-aminomethyl-5-methyl-4H-1,2,4-triazol-4-yl)-benzophenone dihydrobromide (2.3 g) is added under ice cooling and stirring, and the temperature within the flask is gradually returned to room temperature. The reaction mixture is allowed to stand at room temperature, neutralized with saturated aqueous sodium bicarbonate, and shaken with ethyl acetate. The precipitated crystals are filtered, washed with methanol and dried to give 5-chloro-2-[3-(2-phthalimidoacetamidomethyl)-5-methyl-4H-1,2,4-triazol-4-yl]-benzophenone (1.68 g) as crystals melting at 251°-253° C.

Quelle