Reaktion #1933598

ord-5b063da1be2f44889a8c304512d26441

Reaktionsgleichung

COc1ccc2c3c1O[C@H]1C(=O)CC[C@H]4[C@@H](C2)N(C)CC[C@]314.O=C(O)C(O)C(O)C(=O)O
Hydrocodone bitartrate
O=C([O-])O.[Na+]
NaHCO3
→
COc1ccc2c3c1O[C@H]1C(=O)CC[C@H]4[C@@H](C2)N(C)CC[C@]314
hydrocodone

Edukte

COc1ccc2c3c1O[C@H]1C(=O)CC[C@H]4[C@@H](C2)N(C)CC[C@]314.O=C(O)C(O)C(O)C(=O)O
Hydrocodone bitartrate
O=C([O-])O.[Na+]
NaHCO3
—
solid

Reagenzien

Keine

Lösungsmittel

O
water

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeHydrocodone precipitates
  2. 2
    workup.ADDITIONdichlormethane was added
  3. 3
    SonstigeThe layers were then separated
  4. 4
    Extraktionthe basic aqueous layer was extracted two times with dichloromethane
  5. 5
    TrocknenThe organic layer was dried over MgSO4
  6. 6
    Sonstigeevaporated

Vorschrift

Hydrocodone bitartrate salt was dissolved in water. To this was added 2 equivalents solid NaHCO3. Hydrocodone precipitates and dichlormethane was added. The biphasic solution was allowed to stir for twenty minutes. The layers were then separated and the basic aqueous layer was extracted two times with dichloromethane. The organic layer was dried over MgSO4 and evaporated to yield hydrocodone free base as a white powder. Isolated yield was generally 95+%

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08952032B2uspto-grants-2015_02