Реакция #54220

Уравнение реакции

3-(Nα -carbobenzoxyglycyl-glycylamino)-4-hydroxy-4-phenyl-6-chloro-3,4-dihydroquinazoline

→

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

Выход 35.6%

Растворители

acetic acid

Условия реакции

Обработка

1. 1
   Температураwith heating for 2 hours
2. 2
   ДругоеThe reaction mixture is evaporated under reduced pressure
3. 3
   workup.DISSOLUTIONthe residue is dissolved in ethyl acetate (30 ml)
4. 4
   ПромывкаThe ethyl acetate layer is washed with aqueous sodium bicarbonate and water 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 ethyl acetate/methanol

Методика

A solution of 3-(Nα -carbobenzoxyglycyl-glycylamino)-4-hydroxy-4-phenyl-6-chloro-3,4-dihydroquinazoline (1.5 g) in acetic acid (20 ml) is refluxed with heating for 2 hours. The reaction mixture is evaporated under reduced pressure, and the residue is dissolved in ethyl acetate (30 ml). The ethyl acetate layer is washed with aqueous sodium bicarbonate and water 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 ethyl acetate/methanol to give 5-chloro-2-[3-(N-carbobenzoxyglycyl)aminomethyl-4H-1,2,4-triazol-4-yl]-benzophenone as a colorless oil (0.515 g).

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