반응 #54220

반응 방정식

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

수율 35.6%

용매

acetic acid

반응 조건

후처리

1. 1
   온도with heating for 2 hours
2. 2
   기타The reaction mixture is evaporated under reduced pressure
3. 3
   workup.DISSOLUTIONthe residue is dissolved in ethyl acetate (30 ml)
4. 4
   세척The ethyl acetate layer is washed with aqueous sodium bicarbonate and water in order
5. 5
   건조dried over sodium sulfate
6. 6
   기타evaporated under reduced pressure
7. 7
   기타to remove the solvent
8. 8
   기타The residue is chromatographed on a column of silica gel, which
9. 9
   세척is eluted with ethyl acetate/methanol

실험 절차

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).

출처