Reaktion #54221

Reaktionsgleichung

5-chloro-2-[3-(N-carbobenzoxyglycyl)aminomethyl- 4H-1,2,4-triazol-4-yl]-benzophenone

ether

→

5-chloro-2-(3-glycylaminomethyl-4H-1,2,4-triazol-4-yl)-benzophenone

Ausbeute 25.3%

Lösungsmittel

anisole

hydrogen bromide acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe precipitate is filtered
2. 2
   Waschenwashed with ether
3. 3
   workup.DISSOLUTIONdissolved in methylene chloride (20 ml)
4. 4
   WaschenThe methylene chloride layer is washed with saturated aqueous sodium bicarbonate, water and saturated aqueous saline solution in order
5. 5
   Trocknendried over sodium sulfate
6. 6
   Sonstigeevaporated under reduced pressure
7. 7
   Sonstigeto remove the solvent
8. 8
   SonstigeThe residue is chromatographed on a column of silica gel, which
9. 9
   Waschenis eluted with methanol

Vorschrift

To a solution of 5-chloro-2-[3-(N-carbobenzoxyglycyl)aminomethyl- 4H-1,2,4-triazol-4-yl]-benzophenone (2.1 g) in anisole (4 ml), 30% hydrogen bromide-acetic acid is added. The resultant mixture is stirred for 1 hour and mixed with ether. The precipitate is filtered, washed with ether and dissolved in methylene chloride (20 ml). The methylene chloride layer is washed with saturated aqueous sodium bicarbonate, water and saturated aqueous saline solution in order, dried over sodium sulfate and evaporated under reduced pressure to remove the solvent. The residue is chromatographed on a column of silica gel, which is eluted with methanol to give 5-chloro-2-(3-glycylaminomethyl-4H-1,2,4-triazol-4-yl)-benzophenone as a colorless oil (0.39 g).

Quelle