Bazedoxifene Acetate → Bazedoxifene

HRID 1503311

Reaktionsgleichung

Reaktionsgleichung von HRID 1503311
[CH3:1][C:2]1[C:3]2[CH:4]=[C:5]([OH:35])[CH:6]=[CH:7][C:8]=2[N:9]([CH2:18][C:19]2[CH:20]=[CH:21][C:22]([O:25][CH2:26][CH2:27][N:28]3[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]3)=[CH:23][CH:24]=2)[C:10]=1[C:11]1[CH:12]=[CH:13][C:14]([OH:17])=[CH:15][CH:16]=1.CC(O)=O>CN(C)C=O>[CH3:1][C:2]1[C:3]2[CH:4]=[C:5]([OH:35])[CH:6]=[CH:7][C:8]=2[N:9]([CH2:18][C:19]2[CH:24]=[CH:23][C:22]([O:25][CH2:26][CH2:27][N:28]3[CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34]3)=[CH:21][CH:20]=2)[C:10]=1[C:11]1[CH:12]=[CH:13][C:14]([OH:17])=[CH:15][CH:16]=1

Komponenten

3

Edukt 1

HCID 154256Bazedoxifene Acetate

Produkt 1

HCID 154257BazedoxifeneAusbeute 75,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
72.5 °C

Versuchsvorschrift

Bazedoxifene acetate (15 g) and dimethylformamide (75 mL) are mixed and heated to 70-75° C. to produce a clear solution, followed by filtration to make it particle free. To the filtrate, toluene (1000 mL), morpholine (1 mL), and water (500 mL) are added and the mixture is cooled to 25-30° C. and stirred overnight. The solid that forms is collected by filtration, washed with toluene (20 mL), and dried under vacuum at 70° C. for 5 hours to afford 10 g of crystalline bazedoxifene free base Form A.

Aufarbeitung

  1. customto produce a clear solution
  2. filtrationfollowed by filtration
  3. additionTo the filtrate, toluene (1000 mL), morpholine (1 mL), and water (500 mL) are added
  4. temperaturethe mixture is cooled to 25-30° C.
  5. filtrationThe solid that forms is collected by filtration
  6. washwashed with toluene (20 mL)
  7. customdried under vacuum at 70° C. for 5 hours

Quellen und Nachweise

ORD-Eintrag
ord-26db185c049d42e98fd7a3967d07ba63
Quelldatensatz
uspto-grants-2015_12
Patentnummer
US09212172B2

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