Reaktion #69151

ord-cc909c6d7bfc4c6f9c479997830e2d7f

Reaktionsgleichung

C=C1CC[C@@]2(O)[C@H]3Cc4ccc(O)c5c4[C@@]2(CCN3CC2CC2)[C@H]1O5.Cl
Nalmefene Hydrochloride
C=C1CC[C@@]2(O)[C@H]3Cc4ccc(O)c5c4[C@@]2(CCN3CC2CC2)[C@H]1O5
Nalmefene
→
C=C1CC[C@@]2(O)[C@H]3Cc4ccc(O)c5c4[C@@]2(CCN3CC2CC2)[C@H]1O5.Cl.O.O
Nalmefene hydrochloride dihydrate

Edukte

C=C1CC[C@@]2(O)[C@H]3Cc4ccc(O)c5c4[C@@]2(CCN3CC2CC2)[C@H]1O5.Cl
Nalmefene Hydrochloride
C=C1CC[C@@]2(O)[C@H]3Cc4ccc(O)c5c4[C@@]2(CCN3CC2CC2)[C@H]1O5
Nalmefene

Reagenzien

Keine

Reaktionsbedingungen

Temperatur
20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISSOLUTIONThe seed did not dissolve
  2. 2
    Sonstigeto crystallize
  3. 3
    SonstigeWhen the cooling ramp was terminated the suspension
  4. 4
    Temperaturwas maintained
  5. 5
    FiltrationThe solid was filtered
  6. 6
    Waschenwashed with acetone (50 ml)
  7. 7
    SonstigeThe wet product was dried overnight under vacuum at 40° C.

Vorschrift

At 50° C., Nalmefene Hydrochloride was added as seeding. The seed did not dissolve and Nalmefene started to crystallize. When the cooling ramp was terminated the suspension was maintained under stirring at 20° C. for 2.5 days. The solid was filtered and washed with acetone (50 ml). The wet product was dried overnight under vacuum at 40° C. yielding 13.2 g of Nalmefene hydrochloride dihydrate (chemical purity 99.74%, water content 8.54% w/w as measured by Karl Fisher titration).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08530495B2uspto-grants-2013_09