Reaktion #1750199

Reaktionsgleichung

acetic acid

brine

doxorubicin

→

doxorubicin

NaCl

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationless than 0.1%, the reaction mixture was filtered through a coarse sintered glass funnel
2. 2
   Sonstigeto remove the beads
3. 3
   SonstigeThe filtered reaction mixture
4. 4
   FiltrationThe red precipitate was filtered through a medium sintered glass funnel
5. 5
   Waschenwashed with water
6. 6
   Trocknendried under vacuum pressure over P2O5

Vorschrift

At six hours the amount of doxorubicin peak was less than 0.1%, the reaction mixture was filtered through a coarse sintered glass funnel to remove the beads. A brine solution (at least 30% w/v) of 1.1 kg NaCl in 3.5 L water was prepared and cooled to 0° C. The filtered reaction mixture was then slowly added to the cooled brine solution with vigorous stirring over 45 minutes. The color of the solution remained red, a blue solution would have indicated that the pH needed adjustment immediately to between 5.8-6.0 by adding acetic acid. The red precipitate was filtered through a medium sintered glass funnel, washed with water and dried under vacuum pressure over P2O5 to yield MeOSuc-βAla-Leu-Ala-Leu-Dox free of any residual doxorubicin.

Quelle