반응 #1994231

ord-c2655b6532bb4961a9ce71e3f14653d2

반응 방정식

Br.COc1ccc2c(c1)[C@]13CCCC[C@@H]1[C@H](C2)N(C)CC3
dextromethorphan HBr
COc1ccc2c(c1)[C@]13CCCC[C@@H]1[C@H](C2)N(C)CC3
Dextromethorphan

시약

없음

용매

반응 조건

온도
77.5°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONslowly adding 1,758 g of AMBERLITE™
  2. 2
    workup.ADDITIONresin with continuous mixing
  3. 3
    온도while cooling down to room temperature
  4. 4
    workup.ADDITIONThe dispersion was mixed for 4 hours and upon completion
  5. 5
    기타before decanting the supernatant
  6. 6
    기타The wet resin complex was then dried in a VWR™ convection oven
  7. 7
    온도maintained 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
    기타to form a uniform mass
  10. 10
    기타The wet mass was then dried at 50° C. in a VWR™ convection oven to the moisture content
  11. 11
    기타The dried granules were then milled through a 40 mesh screen

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08597684B2uspto-grants-2013_12