تفاعل #1583852

ord-b9744a5ffd9446c4ba5d870de37086b8

معادلة التفاعل

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

المتفاعلات

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
77.5°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

The Dextromethorphan Resin Complex was prepared by first dissolving 954 g of dextromethorphan HBr in 8 L 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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09198864B2uspto-grants-2015_12