反应 #1994236

ord-fd8e7d023d64439790e929c82e60ccb4

反应方程式

COc1ccc2c3c1O[C@H]1C(=O)CC[C@H]4[C@@H](C2)N(C)CC[C@]314.O=C(O)C(O)C(O)C(=O)O
hydrocodone Bitartrate
COc1ccc2c3c1O[C@H]1C(=O)CC[C@H]4[C@@H](C2)N(C)CC[C@]314
Hydrocodone

试剂

溶剂

反应条件

温度
50°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONslowly adding 1,407 g of AMBERLITE™
  2. 2
    workup.ADDITIONThe dispersion was mixed for 4 hours and upon completion
  3. 3
    其他before decanting the supernatant
  4. 4
    其他The wet resin complex was then dried in a VWR™ convection oven
  5. 5
    workup.ADDITIONKOLLICOAT™ SR-30D polymer (500 g) was then slowly added to the wet resin complex in a Hobart type mixer (Kitchen Aid)
  6. 6
    其他to form a uniform mass
  7. 7
    其他The wet mass was again dried in a 50° C
  8. 8
    其他The semi-dried granules were then milled through a 40 mesh screen
  9. 9
    其他continued drying under 50° C. until the moisture content
  10. 10
    其他The dried granules were then milled through a 40 mesh screen

实验过程

The Hydrocodone Resin Complex was prepared by first dissolving 450 g of hydrocodone Bitartrate in 8 kg of purified water, and then slowly adding 1,407 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 in a VWR™ convection oven maintained at 50° C. until moisture content was about 20-25%. KOLLICOAT™ SR-30D polymer (500 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™ convection oven to the moisture content around 15-20%. The semi-dried granules were then milled through a 40 mesh screen using CO-MIL™ brand mill and continued drying under 50° C. until the moisture content was between 3-7%. The dried granules were then milled through a 40 mesh screen using CO-MIL™ brand mill.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08597684B2uspto-grants-2013_12