Reaktion #69152

Reaktionsgleichung

Nalmefene hydrochloride

→

Nalmefene hydrochloride dihydrate

Ausbeute 192.7%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISSOLUTIONcompletely dissolved
2. 2
   Sonstigeto remove organic solvents
3. 3
   FiltrationThe resulting solution was then filtered through a 0.65 μm cartridge
4. 4
   workup.ADDITIONdiluted with water (2.1 liter)
5. 5
   Waschento rinse the reactor and pipelines
6. 6
   TemperaturThe solution was cooled down to 50° C.
7. 7
   workup.ADDITION7 g of Nalmefene hydrochloride dihydrate seeding material was added
8. 8
   TemperaturThe mixture was cooled down to 0-5° C. in one hour
9. 9
   Temperaturmaintained
10. 10
    workup.STIRRINGunder stirring for one additional hour
11. 11
    FiltrationThe solid was filtered
12. 12
    Waschenwashed with acetone
13. 13
    SonstigeThe wet product was dried at 25° C. under vacuum

Vorschrift

Crude Nalmefene hydrochloride (7.67 Kg, assay 93.9%) and water (8.6 liter) were charged into a suitable reactor. The suspension was heated up to 80° C. until the substrate completely dissolved. Vacuum was then applied to remove organic solvents. The resulting solution was then filtered through a 0.65 μm cartridge and then diluted with water (2.1 liter) used to rinse the reactor and pipelines. The solution was cooled down to 50° C. and 7 g of Nalmefene hydrochloride dihydrate seeding material was added. The mixture was cooled down to 0-5° C. in one hour under efficient stirring and then maintained under stirring for one additional hour. The solid was filtered and washed with acetone. The wet product was dried at 25° C. under vacuum to provide Nalmefene hydrochloride dihydrate (5.4 Kg; yield 73%) with a chemical purity of 99.89% (HPLC).

Quelle