Dextromethorphan Hydrobromide → Dextromethorphan

HRID 333512

反応式

HRID 333512 の反応式
[CH3:1][N:2]1[C@H:11]2[CH2:12][C:13]3[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][C:14]=3[C@:5]3([C@@H:10]2[CH2:9][CH2:8][CH2:7][CH2:6]3)[CH2:4][CH2:3]1.Br>O>[CH3:1][N:2]1[C@H:11]2[CH2:12][C:13]3[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][C:14]=3[C@:5]3([C@@H:10]2[CH2:9][CH2:8][CH2:7][CH2:6]3)[CH2:4][CH2:3]1

参加物

3

反応条件

温度
77.5 °C

実験手順

The Dextromethorphan Resin Complex was prepared by first dissolving 954 g of dextromethorphan HBr in 8 liters of purified water heated to 75-80° C., and then slowly adding 1,758 g of AMBERLITE™ IRP-69 resin with continuous mixing while cooling down to room temperature. 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%. In a separate container, KOLLIDON K-30 polymer (116 g) was dissolved in 1,150 g of purified water and slowly applied to the wet resin complex in a Hobart type mixer (Kitchen Aid) to form a uniform mass. The wet mass was then dried at 50° C. in a VWR™ convection oven to the moisture content was around 4-6%. The dried granules were then milled through a 40 mesh screen using CO-MIL™ brand mill.

後処理

  1. additionslowly adding 1,758 g of AMBERLITE™
  2. additionresin with continuous mixing
  3. temperaturewhile cooling down to room temperature
  4. additionThe dispersion was mixed for 4 hours and upon completion
  5. custombefore decanting the supernatant
  6. customThe wet resin complex was then dried in a VWR™ convection oven
  7. temperaturemaintained at 50° C. until moisture content
  8. dissolutionIn a separate container, KOLLIDON K-30 polymer (116 g) was dissolved in 1,150 g of purified water
  9. customto form a uniform mass
  10. customThe wet mass was then dried at 50° C. in a VWR™ convection oven to the moisture content
  11. customThe dried granules were then milled through a 40 mesh screen

出典と根拠

ORDレコード
ord-63b39d2f6cb44373bc48062043d99df2
出典データセット
uspto-grants-2014_11
特許番号
US08883217B2

関連ノート

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