Oxybutynin hydrochloride → Oxybutynin

HRID 403104Notes

Reaction equation

HRID 403104 reaction equation
[CH3:1][CH2:2][N:3]([CH2:6][C:7]#[C:8][CH2:9][O:10][C:11]([C:13]([OH:26])([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH:14]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1)=[O:12])[CH2:4][CH3:5].Cl>O>[CH3:1][CH2:2][N:3]([CH2:6][C:7]#[C:8][CH2:9][O:10][C:11]([C:13]([OH:26])([CH:20]1[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25]1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=[O:12])[CH2:4][CH3:5]

Participants

3

Reactant 1

HCID 91505Oxybutynin hydrochloride

Product 1

HCID 4634Oxybutynin

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
50 °C

Procedure

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-MIL™.

Workup

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

Sources & evidence

ORD record
ord-3bc703093ae94171b5da6cf17c2311c3
Source dataset
uspto-grants-2014_06
Patent number
US08747902B2

Reaction notes

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