反应 #1994234

ord-db0b4aa6300c47f4b990a9e807bd61a3

反应方程式

CN[C@@H](C)[C@@H](O)c1ccccc1.Cl
pseudoephedrine HCl
CN[C@@H](C)[C@@H](O)c1ccccc1
Pseudoephedrine

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 1,589 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
    过滤The slurry was filtered
  5. 5
    洗涤rinsed 3 times with sufficient amounts of purified water
  6. 6
    其他The wet resin complex was then dried in a VWR™ convection oven
  7. 7
    workup.ADDITIONKOLLICOAT™ SR-30D polymer (668 g) was then slowly added to the wet resin complex in a Hobart type mixer (Kitchen Aid)
  8. 8
    其他to form a uniform mass
  9. 9
    其他The wet mass was again dried at 50° C. in a VWR™ convection oven to the moisture content around 30%
  10. 10
    其他The semi-dried granules were then milled through a 40 mesh screen
  11. 11
    其他continued drying under 50° C. until the moisture content
  12. 12
    其他The dried granules were then milled through a 40 mesh screen

实验过程

The Pseudoephedrine Resin Complex was prepared by first dissolving 857 g of pseudoephedrine HCl in 5 liter of purified water, and then slowly adding 1,589 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 slurry was filtered and rinsed 3 times 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 25%. KOLLICOAT™ SR-30D polymer (668 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 at 50° C. in a VWR™ convection oven to the moisture content around 30%. 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 4-6%. 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