Diethyl Ether → Quetiapine Besylate

HRID 421568

Reaktionsgleichung

Reaktionsgleichung von HRID 421568
[CH:1]1[CH:2]=[CH:3][C:4]2[S:15][C:14]3[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=3[N:8]=[C:7]([N:16]3[CH2:21][CH2:20][N:19]([CH2:22][CH2:23][O:24][CH2:25][CH2:26][OH:27])[CH2:18][CH2:17]3)[C:5]=2[CH:6]=1.[C:28]1([S:34]([OH:37])(=[O:36])=[O:35])[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.C(OCC)C>CC(C)=O>[CH:1]1[CH:2]=[CH:3][C:4]2[S:15][C:14]3[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=3[N:8]=[C:7]([N:16]3[CH2:21][CH2:20][N:19]([CH2:22][CH2:23][O:24][CH2:25][CH2:26][OH:27])[CH2:18][CH2:17]3)[C:5]=2[CH:6]=1.[S:34]([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)([O-:37])(=[O:36])=[O:35]

Komponenten

5

Edukt 3

HCID 3283Diethyl EtherHCID 5002QuetiapineHCID 7371Benzenesulfonic Acid

Produkt 1

HCID 131729401Quetiapine Besylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Reaktionsbedingungen

Temperatur
42.5 °C

Versuchsvorschrift

Quetiapine free base (5.0 g) was dissolved in acetone (50 ml) at room temperature. This was followed by the addition of benzene sulfonic acid (2.0 g) at 30 to 35° C. The resulting mass was heated at 40-45° C. and maintained for 30 minutes. The resulting mass was cooled at 25-30° C. This was followed by the addition of diethyl ether (50 ml) and stirred for 3 hours. The precipitated product was collected by filtration under nitrogen and washed with diethyl ether (25 ml) and dried under vacuum to give the title compound as off white powder (5.94 g).

Aufarbeitung

  1. temperaturemaintained for 30 minutes
  2. temperatureThe resulting mass was cooled at 25-30° C
  3. filtrationThe precipitated product was collected by filtration under nitrogen
  4. washwashed with diethyl ether (25 ml)
  5. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-c659196a311943ae9e9e81e03e4b6e1a
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08101597B2

Verknüpfte Notizen

Wird geladen…