Reaktion #1437784

ord-43810e51ab6145628b3b2eab9ae8e0d2

Reaktionsgleichung

CC(=O)O
acetic acid
O.[Cl-].[Na+]
brine
COc1cccc2c1C(=O)c1c(O)c3c(c(O)c1C2=O)C[C@@](O)(C(=O)CO)C[C@@H]3O[C@H]1C[C@H](N)[C@H](O)[C@H](C)O1
doxorubicin
COc1cccc2c1C(=O)c1c(O)c3c(c(O)c1C2=O)C[C@@](O)(C(=O)CO)C[C@@H]3O[C@H]1C[C@H](N)[C@H](O)[C@H](C)O1
doxorubicin
[Cl-].[Na+]
NaCl

Reagenzien

Keine

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

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

Vorschrift

When the doxorubicin peak is less than 0.1%, the reaction mixture is 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 is prepared and cooled to 0° C. The filtered reaction mixture is then slowly added to the cooled brine solution with vigorous stirring over 45 minutes. The color of the solution must remain red, a blue solution indicates that the pH needs adjustment immediately to between 5.8–6.0 by adding acetic acid. The red precipitate is filtered through a medium sintered glass funnel, washed with water and dried under vacuum pressure over P2O5 to yield MeOSuc-Leu-Ala-Leu-Dox free of any residual doxorubicin.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07214663B2uspto-grants-2007_05