Reaction #1994241

ord-b256c166a61b406190061437fd0ef475

Reaction equation

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

Reactants

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

Reagents

None

Solvents

O
water

Conditions

Temperature
77.5°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    workup.ADDITIONfollowed by the addition of 175.82 g AMBERLITE IRP-69 resin (anhydrous)
  2. 2
    workup.ADDITIONunder gentle mixing for 4 hours
  3. 3
    Otherdecanted
  4. 4
    Washrinsed with purified water twice
  5. 5
    Otherdried in an oven
  6. 6
    Temperaturemaintained at 50° C. until moisture
  7. 7
    Filtrationsieved through a 40 mesh screen

Procedure

The Uncoated Dextromethorphan Resin Complex was prepared by first dissolving 95.42 g of dextromethorphan HBr in 0.8 L of purified water heated to 75-80° C., followed by the addition of 175.82 g AMBERLITE IRP-69 resin (anhydrous) under gentle mixing for 4 hours. At the completion, the suspension was allowed to settle, decanted and rinsed with purified water twice and dried in an oven maintained at 50° C. until moisture is around 5%. The dried resin complex was hand sieved through a 40 mesh screen.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08597684B2uspto-grants-2013_12