Reaktion #1994238

ord-b67d0e85caea48cea4ac7270ab804c70

Reaktionsgleichung

CCN(CC)CC#CCOC(=O)C(O)(c1ccccc1)C1CCCCC1.Cl
oxybutynin hydrochloride
CCN(CC)CC#CCOC(=O)C(O)(c1ccccc1)C1CCCCC1
Oxybutynin

Reagenzien

Keine

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONslowly adding 1586 g of AMBERLITE™
  2. 2
    workup.ADDITIONThe dispersion was mixed for 4 hours
  3. 3
    Sonstigebefore decanting the supernatant
  4. 4
    SonstigeThe wet resin complex was then dried in a VWR™ convention oven
  5. 5
    workup.ADDITIONKOLLICOAT™ SR-30D polymer system (540 g) was then slowly added to the wet resin complex in a Hobart type mixer (Kitchen Aid)
  6. 6
    Sonstigeto form a uniform mass
  7. 7
    SonstigeThe wet mass was again dried in a 50° C
  8. 8
    SonstigeThe semi-dried granules were then milled through a 40 mesh screen
  9. 9
    Sonstigecontinued drying at 50° C. until the moisture content
  10. 10
    SonstigeThe dried granules were then milled through a 40 mesh screen

Vorschrift

The Oxybutynin Resin Complex was prepared by first dissolving 300 g of oxybutynin hydrochloride in 8 L of purified water, and then slowly adding 1586 g of AMBERLITE™ IRP-69 resin with continuous mixing. The pH was adjusted to 3.9. 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™ convention oven maintained at 50° C. until moisture content was about 25%. KOLLICOAT™ SR-30D polymer system (540 g) was then slowly added to the wet resin complex in a Hobart type mixer (Kitchen Aid) to form a uniform mass. The wet mass was again dried in a 50° C. VWR™ convention oven to the moisture content about 25%. The semi-dried granules were then milled through a 40 mesh screen using CO-MIL™ and continued drying at 50° C. until the moisture content was between 3-7%. The dried granules were then milled through a 40 mesh screen using CO-MILT™.

Quelle

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