Реакция #54221

Уравнение реакции

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

Выход 25.3%

Растворители

anisole

hydrogen bromide acetic acid

Условия реакции

Обработка

1. 1
   ФильтрацияThe precipitate is filtered
2. 2
   Промывкаwashed with ether
3. 3
   workup.DISSOLUTIONdissolved in methylene chloride (20 ml)
4. 4
   ПромывкаThe methylene chloride layer is washed with saturated aqueous sodium bicarbonate, water and saturated aqueous saline solution in order
5. 5
   Сушкаdried over sodium sulfate
6. 6
   Другоеevaporated under reduced pressure
7. 7
   Другоеto remove the solvent
8. 8
   ДругоеThe residue is chromatographed on a column of silica gel, which
9. 9
   Промывкаis eluted with methanol

Методика

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).

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