Isopropanol → Desvenlafaxine fumarate

HRID 561725

반응식

HRID 561725 반응식
[CH3:1][N:2]([CH2:4][CH:5]([C:13]1([OH:19])[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1)[C:6]1[CH:7]=[CH:8][C:9]([OH:12])=[CH:10][CH:11]=1)[CH3:3].[C:20]([OH:27])(=[O:26])/[CH:21]=[CH:22]/[C:23]([OH:25])=[O:24].C(O)(C)C>C(OCC)(=O)C(C)O>[CH3:1][N:2]([CH2:4][CH:5]([C:13]1([OH:19])[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1)[C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1)[CH3:3].[CH:21](/[C:20]([OH:27])=[O:26])=[CH:22]\[C:23]([OH:25])=[O:24]

참가 물질

5

반응물 3

HCID 3776Isopropanol2회HCID 125017Desvenlafaxine2회HCID 444972Fumaric Acid2회

생성물 1

HCID 13520322Desvenlafaxine fumarate

시약·촉매·용매 1

HCID 7344Ethyl Lactate용매

실험 절차

In one specific embodiment, O-desmethylvenlafaxine, fumaric acid and the isopropyl alcohol or ethyl lactate solvent are combined to form a solution. Where the solvent is isopropyl alcohol, O-desmethylvenlafaxine and fumaric acid in the solvent may be heated to obtain a solution. Heating may be carried out from about room temperature to about reflux temperature of the solvent. The solution may than be cooled to a temperature of about 50° C. or less, preferably to about 15° C. to about 30° C., preferably to about room temperature. The solution is maintained for an overnight period, preferably about 8 hours to about 20 hours, more preferably for about 18 hours, at a temperature of about 15° C. to about 30° C., preferably room temperature, to obtain O-desmethylvenlafaxine fumarate crystal Form II. The reaction mixture may be stirred before, during or after precipitation.

후처리

  1. customto form a solution
  2. temperaturemay be heated
  3. customto obtain a solution
  4. temperatureHeating may
  5. custombe carried out from about room temperature
  6. temperatureto about reflux temperature of the solvent
  7. temperatureThe solution may than be cooled to a temperature of about 50° C. or less, preferably to about 15° C. to about 30° C., preferably to about room temperature

출처 및 근거

ORD 기록
ord-738572a2d3bc48669b4476d0bb6413c6
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063250B2

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