Reaktion #11900

Reaktionsgleichung

toluene

trityl candesartan cilexetil

formic acid

→

candesartan cilexetil

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturTypically, the deprotection step comprises heating
2. 2
   Temperaturto reflux until a clear solution
3. 3
   Sonstigeis obtained
4. 4
   Sonstigeis from about 30° C. to about 90° C., preferably from about 50° C. to about 90° C.
5. 5
   Sonstigefor about 5 to about 19 hours
6. 6
   workup.WAITpreferably for about 8 to about 12 hours
7. 7
   SonstigeThereafter, the solvents are removed by evaporation

Vorschrift

Typically, the deprotection step comprises heating to reflux trityl candesartan cilexetil in methanol. Optionally, the deprotection solvent mixture further comprises an organic solvent, such as toluene, and/or an acid, such as formic acid. The cilexetil trityl candesartan is heated to reflux until a clear solution is obtained. Typically, the reaction temperature is from about 30° C. to about 90° C., preferably from about 50° C. to about 90° C., and the heating takes place for about 5 to about 19 hours, preferably for about 8 to about 12 hours. Thereafter, the solvents are removed by evaporation to obtain crude deprotected candesartan cilexetil. The solvents may be removed at a temperature of about 30° C. to about 70° C., preferably at a temperature of about 50° C., and at a reduce pressure of about 30 mbar.

Quelle