Acetone → Solifenacin Succinate

HRID 1616251

反応式

HRID 1616251 の反応式
CC(C)=O.[C:5]([OH:12])(=[O:11])[CH2:6][CH2:7][C:8]([OH:10])=[O:9].[CH:13]1[CH:14]=[CH:15][C:16]([C@@H:19]2[N:28]([C:29]([O:31][C@@H:32]3[CH:37]4[CH2:38][CH2:39][N:34]([CH2:35][CH2:36]4)[CH2:33]3)=[O:30])[CH2:27][CH2:26][C:25]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]2=3)=[CH:17][CH:18]=1>O>[CH:13]1[CH:18]=[CH:17][C:16]([C@@H:19]2[N:28]([C:29]([O:31][C@@H:32]3[CH:37]4[CH2:36][CH2:35][N:34]([CH2:39][CH2:38]4)[CH2:33]3)=[O:30])[CH2:27][CH2:26][C:25]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]2=3)=[CH:15][CH:14]=1.[CH2:6]([C:5]([OH:12])=[O:11])[CH2:7][C:8]([OH:10])=[O:9]

参加物

5

反応物 3

HCID 180AcetoneHCID 1110Succinic AcidHCID 154059Solifenacin

生成物 1

HCID 216457Solifenacin Succinate

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
3 °C

実験手順

Acetone (260 ml), Succinic acid (12.7 g, 0.107 mol) and water (5 ml) are combined in a flask. The mixture is heated under reflux until total dissolution and then kept at 42° C. Then, the “Solution of solifenacin base” is charged and the mixture is heated to reflux and kept under reflux for 15 minutes. The content is distilled until a final volume of 260 ml. The mixture is cooled slowly until a final temperature of 3° C. and then filtered. The residue is washed with Ethyl acetate (50 ml) at 0/5° C. and is drained for 1 hour. The wet cake is dried in the vacuum oven at 60° C. to give a white solid.

後処理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux until total dissolution
  3. customkept at 42° C
  4. temperaturethe mixture is heated
  5. temperatureto reflux
  6. temperatureunder reflux for 15 minutes
  7. distillationThe content is distilled until a final volume of 260 ml
  8. filtrationfiltered
  9. washThe residue is washed with Ethyl acetate (50 ml) at 0/5° C.
  10. customThe wet cake is dried in the vacuum oven at 60° C.
  11. customto give a white solid

出典と根拠

ORDレコード
ord-a0974220dcd9492396cd4fe3c5c1e2cc
出典データセット
uspto-grants-2014_07
特許番号
US08765785B2

関連ノート

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