반응 #81263

반응 방정식

water

(5-methyl-2-oxo-1,3-dioxolen-4-yl)methyl 4-(1-hydroxy-1-methylethyl)-2-propyl-1-{4-[2-(trityltetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate

water

→

title compound

수율 81.2%

(5-Methyl-2-oxo-1,3-dioxolen-4-yl)methyl 4-(1-hydroxy-1-methylethyl)-2-propyl-1-{4-[2-(tetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate

수율 81.2%

용매

acetic acid

반응 조건

후처리

1. 1
   온도was then cooled
2. 2
   기타Precipitated trityl alcohol was removed by filtration
3. 3
   농축the filtrate was concentrated by evaporation under reduced pressure
4. 4
   workup.ADDITIONToluene was added to the residue
5. 5
   농축the mixture was again concentrated by evaporation under reduced pressure
6. 6
   기타to remove the remaining water and acetic acid
7. 7
   기타The residue was crystallized in ethyl acetate

실험 절차

75 ml of water were added to a suspension of 29.3 g of (5-methyl-2-oxo-1,3-dioxolen-4-yl)methyl 4-(1-hydroxy-1-methylethyl)-2-propyl-1-{4-[2-(trityltetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate [prepared as described in step (a) above] in 225 ml of acetic acid, and the resulting mixture was stirred at 60° C. for 1.5 hours. At the end of this time, 75 ml of water were added to the mixture, which was then cooled. Precipitated trityl alcohol was removed by filtration, and the filtrate was concentrated by evaporation under reduced pressure. Toluene was added to the residue, and the mixture was again concentrated by evaporation under reduced pressure, to remove the remaining water and acetic acid. The residue was crystallized in ethyl acetate, to give 16.6 g of the title compound as crystals, melting at 177°-180° C. (with decomposition).

출처