Hydrochloric Acid → Oxycodone Hydrochloride

HRID 84140

Reaktionsgleichung

Reaktionsgleichung von HRID 84140
[CH3:1][N:2]1[C@@H:19]2[CH2:20][C:7]3[CH:8]=[CH:9][C:10]([O:22][CH3:23])=[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]=34)[CH2:4][CH2:3]1)=[O:15].[ClH:24].CC(O)C>O.C(O)(=O)C>[CH3:1][N:2]1[C@@H:19]2[CH2:20][C:7]3[CH:8]=[CH:9][C:10]([O:22][CH3:23])=[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]=34)[CH2:4][CH2:3]1)=[O:15].[ClH:24]

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 5284603Oxycodone

Produkt 1

HCID 5462350Oxycodone HydrochlorideAusbeute 93 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

The first portion of purified Oxycodone base lot P (13.56 g, 43.0 mmol) was dissolved (in 80-mL beaker over 15 minutes) in a mixture of water (13 mL) and acetic acid (3 mL). Hydrochloric acid (10.41 mol/kg, 5.0 g, or 51.6 mmol) was added to the solution over 5 minutes. Stirring was continued for another 40 minutes and IPA (55 mL) was added over 15 minutes. Stirring was continued for another 30 minutes. Precipitated product was filtered off, washed on filter with IPA (2×20 ml) and acetone (2×20 mL), dried on filter providing 14.74 g oxycodone HCl (39.86 mmol, 93% yield on OC base purified) lot Q.

Aufarbeitung

  1. stirringStirring
  2. waitwas continued for another 30 minutes
  3. filtrationPrecipitated product was filtered off
  4. washwashed
  5. filtrationon filter with IPA (2×20 ml) and acetone (2×20 mL)
  6. customdried
  7. filtrationon filter

Quellen und Nachweise

ORD-Eintrag
ord-c9088e28dfee4bb9a1438e5d7e3db7c5
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08846923B1

Verknüpfte Notizen

Wird geladen…