Reaktion #81293

Reaktionsgleichung

ethyl 4-(1-hydroxy-1-methylethyl)-2-methylthio-1-{4-[2-(trityltetrazol-5-yl)phenyl]phenyl}metylimidazole-5-carboxylate

→

title compound

Ausbeute 88.5%

Ethyl 4-(1-hydroxy-1-methylethyl)-2-methylthio-1-{4-[2-(tetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate

Ausbeute 88.5%

Lösungsmittel

acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAt the end of this time, the reaction mixture was cooled
2. 2
   Filtrationthe crystals of trityl alcohol which appeared were filtered off
3. 3
   WaschenThese crystals were washed with a 50% v/v aqueous solution of acetic acid
4. 4
   workup.ADDITIONthe filtrate and the washings were mixed
5. 5
   EinengenThe resulting mixture was concentrated by evaporation under reduced pressure
6. 6
   Sonstigethe resulting residue was crystallized from ethyl acetate

Vorschrift

900 mg of ethyl 4-(1-hydroxy-1-methylethyl)-2-methylthio-1-{4-[2-(trityltetrazol-5-yl)phenyl]phenyl}metylimidazole-5-carboxylate [prepared as described in step (a) above] were added to 10 ml of a 25% v/v aqueous solution of acetic acid, and the mixture was stirred at 60° C. for 1 hour. At the end of this time, the reaction mixture was cooled, and the crystals of trityl alcohol which appeared were filtered off. These crystals were washed with a 50% v/v aqueous solution of acetic acid, and the filtrate and the washings were mixed. The resulting mixture was concentrated by evaporation under reduced pressure, and the resulting residue was crystallized from ethyl acetate, to give 529 mg of the title compound as crystals, melting at 209°-210° C.

Quelle