반응 #11900

반응 방정식

toluene

trityl candesartan cilexetil

formic acid

→

candesartan cilexetil

용매

methanol

반응 조건

후처리

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

실험 절차

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.

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