Hydrochloric Acid → Venlafaxine Hydrochloride

HRID 20621

反応式

HRID 20621 の反応式
[CH3:1][N:2]([CH2:4][CH:5]([C:14]1([OH:20])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1)[C:6]1[CH:7]=[CH:8][C:9]([O:12][CH3:13])=[CH:10][CH:11]=1)[CH3:3].C(OC(C)C)(=O)C.[ClH:28]>>[CH3:1][N:2]([CH2:4][CH:5]([C:14]1([OH:20])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1)[C:6]1[CH:7]=[CH:8][C:9]([O:12][CH3:13])=[CH:10][CH:11]=1)[CH3:3].[ClH:28]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 5656VenlafaxineHCID 7915Isopropyl Acetate

生成物 1

HCID 62923Venlafaxine Hydrochloride収率 88%

実験手順

To the solution of venlafaxine base in isopropyl acetate from example 1 (66 ml, 10 mmol) 5 ml of 2 M aqueous HCl were added. The mixture was heated and water was removed by azeotropic distillation using a Dean-Starck trap. When all water was removed from the mixture, the product began slowly to crystallize. The obtained suspension was heated under reflux temperature for 1.5 h, then cooled and filtered. 2.75 g (88% from N,N-didesmethyl venlafaxine hydrochloride) of pure venlafaxine hydrochloride form I (HPLC: 99.65 area %) were obtained.

後処理

  1. temperatureThe mixture was heated
  2. customwater was removed by azeotropic distillation
  3. customWhen all water was removed from the mixture
  4. customto crystallize
  5. temperatureThe obtained suspension was heated
  6. temperatureunder reflux temperature for 1.5 h
  7. temperaturecooled
  8. filtrationfiltered

出典と根拠

ORDレコード
ord-b19b7219e7da48a7bfb6ddb406b91cc9
出典データセット
uspto-grants-2010_06
特許番号
US07745664B2

関連ノート

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