Codeine phosphate hydrate → Codeine

HRID 219485Notes

Reaction equation

HRID 219485 reaction equation
[CH3:1][N:2]1[C@@H:18]2[CH2:19][C:7]3[CH:8]=[CH:9][C:10]([O:21][CH3:22])=[C:11]4[O:12][C@H:13]5[C@@H:14]([OH:20])[CH:15]=[CH:16][C@@H:17]2[C@:5]5([C:6]=34)[CH2:4][CH2:3]1.O.OP(O)(O)=O>O>[CH3:1][N:2]1[C@@H:18]2[CH2:19][C:7]3[CH:8]=[CH:9][C:10]([O:21][CH3:22])=[C:11]4[O:12][C@H:13]5[C@@H:14]([OH:20])[CH:15]=[CH:16][C@@H:17]2[C@:5]5([C:6]=34)[CH2:4][CH2:3]1

Participants

3

Reactant 1

HCID 9953630Codeine phosphate hydrate

Product 1

HCID 5284371Codeine

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
50 °C

Procedure

The Codeine Resin Complex was prepared by first dissolving 500 g of codeine phosphate in 5 kg of purified water, and then slowly adding 1,856 g of AMBERLITE™ IRP-69 resin with continuous mixing. 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 at VWR™ convection oven maintained at 50° C. until moisture content was about 20-30%. EUDRAGIT™ NE-30D polymer system (668 g) was mixed with 1,150 g of purified water and then slowly added to the wet resin complex in a Hobart type mixer (Kitchen Aid) to form a uniform mass. The wet mass was dried at 50° C. in a VWR™ convection oven to the moisture content around 3-7%. The dried granules were then milled through 40 mesh screen using CO-MIL™ brand mill.

Workup

  1. additionslowly adding 1,856 g of AMBERLITE™
  2. additionThe dispersion was mixed for 4 hours and upon completion
  3. custombefore decanting the supernatant
  4. customThe wet resin complex was then dried at VWR™ convection oven
  5. additionEUDRAGIT™ NE-30D polymer system (668 g) was mixed with 1,150 g of purified water
  6. additionslowly added to the wet resin complex in a Hobart type mixer (Kitchen Aid)
  7. customto form a uniform mass
  8. customThe wet mass was dried at 50° C. in a VWR™ convection oven to the moisture content around 3-7%
  9. customThe dried granules were then milled through 40 mesh screen

Sources & evidence

ORD record
ord-467132274e144c53937ff22022ff05b0
Source dataset
uspto-grants-2012_06
Patent number
US08202537B2

Reaction notes

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