반응 #2124096

ord-502f626a61aa4f03854e331547b35fba

반응 방정식

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

반응물

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

시약

없음

용매

O
water

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Hydrocodone precipitates
  2. 2
    workup.ADDITIONdichlormethane was added
  3. 3
    기타The layers were then separated
  4. 4
    추출the basic aqueous layer was extracted two times with dichloromethane
  5. 5
    건조The organic layer was dried over MgSO4
  6. 6
    기타evaporated

실험 절차

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+%

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08575196B2uspto-grants-2013_11