Hydrochloric Acid → Oxymorphone Hydrochloride

HRID 1094626Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1094626
[CH3:1][N:2]1[C@@H:19]2[CH2:20][C:7]3=[CH:8][CH:9]=[C:10]([OH:22])[C:11]4[O:12][C@H:13]5[C:14]([CH2:16][CH2:17][C@:18]2([OH:21])[C@:5]5([C:6]=43)[CH2:4][CH2:3]1)=[O:15].[ClH:23]>C(O)C>[CH3:1][N:2]1[C@@H:19]2[CH2:20][C:7]3=[CH:8][CH:9]=[C:10]([OH:22])[C:11]4[O:12][C@H:13]5[C:14]([CH2:16][CH2:17][C@:18]2([OH:21])[C@:5]5([C:6]=43)[CH2:4][CH2:3]1)=[O:15].[ClH:23]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 5284604Oxymorphone

Produkt 1

HCID 5359390Oxymorphone HydrochlorideAusbeute 86,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
55 °C

Versuchsvorschrift

Purified oxymorphone (17.8 g, 59 mmol) is suspended in 94% aq. ethanol (107 ml) and stirred at 50-60° C. Concentrated hydrochloric acid (32%) is added slowly to adjust the pH to 2.58. The mixture is allowed to cool to room temperature, and then cooled further to 0-10° C., stirred for 2 hours and filtered then washed with ethanol (3×20 ml). The isolated solids are dried at 75° C. under 25 inches-Hg overnight to give oxymorphone HCl as white solids (17.3 g, 51 mmol, 86.7% yield).

Aufarbeitung

  1. temperatureto cool to room temperature
  2. temperaturecooled further to 0-10° C.
  3. stirringstirred for 2 hours
  4. filtrationfiltered
  5. washthen washed with ethanol (3×20 ml)
  6. customThe isolated solids are dried at 75° C. under 25 inches-Hg overnight

Quellen und Nachweise

ORD-Eintrag
ord-84af20b7880c4433a660dba06691702a
Quelldatensatz
uspto-grants-2012_03
Patentnummer
US08134002B2

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