Hydrochloric Acid → Venlafaxine Hydrochloride

HRID 13747

반응식

HRID 13747 반응식
[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]

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 5656VenlafaxineHCID 7915Isopropyl Acetate

생성물 1

HCID 62923Venlafaxine Hydrochloride수율 88%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cc2d78d90b8e409797f0287cfb492f5b
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728173B2

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