Reaktion #1994231

Reaktionsgleichung

dextromethorphan HBr

→

Dextromethorphan

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONslowly adding 1,758 g of AMBERLITE™
2. 2
   workup.ADDITIONresin with continuous mixing
3. 3
   Temperaturwhile cooling down to room temperature
4. 4
   workup.ADDITIONThe dispersion was mixed for 4 hours and upon completion
5. 5
   Sonstigebefore decanting the supernatant
6. 6
   SonstigeThe wet resin complex was then dried in a VWR™ convection oven
7. 7
   Temperaturmaintained at 50° C. until moisture content
8. 8
   workup.DISSOLUTIONIn a separate container, KOLLIDON K-30 polymer (116 g) was dissolved in 1,150 g of purified water
9. 9
   Sonstigeto form a uniform mass
10. 10
    SonstigeThe wet mass was then dried at 50° C. in a VWR™ convection oven to the moisture content
11. 11
    SonstigeThe dried granules were then milled through a 40 mesh screen

Vorschrift

The Dextromethorphan Resin Complex was prepared by first dissolving 954 g of dextromethorphan HBr in 8 liters of purified water heated to 75-80° C., and then slowly adding 1,758 g of AMBERLITE™ IRP-69 resin with continuous mixing while cooling down to room temperature. The dispersion was mixed for 4 hours and upon completion, allowed to settle before decanting the supernatant. The slurring/decanting process was repeated twice with sufficient amounts of purified water. The wet resin complex was then dried in a VWR™ convection oven maintained at 50° C. until moisture content was about 20-25%. In a separate container, KOLLIDON K-30 polymer (116 g) was dissolved in 1,150 g of purified water and slowly applied to the wet resin complex in a Hobart type mixer (Kitchen Aid) to form a uniform mass. The wet mass was then dried at 50° C. in a VWR™ convection oven to the moisture content was around 4-6%. The dried granules were then milled through a 40 mesh screen using CO-MIL™ brand mill.

Quelle