Sulfuric Acid → HCID 86647093, Verbindung

HRID 421565

Reaktionsgleichung

Reaktionsgleichung von HRID 421565
[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:28](=[O:32])(=[O:31])([OH:30])[OH:29]>C(O)(C)C>[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:28]([O-:32])([O-:31])(=[O:30])=[O:29]

Komponenten

4

Edukt 2

HCID 1118Sulfuric AcidHCID 5002Quetiapine

Produkt 1

HCID 86647093HCID 86647093, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Reaktionsbedingungen

Temperatur
27.5 °C

Versuchsvorschrift

Quetiapine free base (5.0 g) was dissolved in isopropyl alcohol (50 ml) at room temperature. This was followed by addition of 98% sulfuric acid (1.28 g) at 30 to 35° C. The resulting gummy mass was heated to reflux and maintained for 15 minutes. The resulting mass was cooled at 25-30° C. and stirred for 1 hour. The precipitated product was collected by filtration, washed with isopropyl alcohol (25 ml) and dried to give the title compound as off white powder (5.88 g).

Aufarbeitung

  1. temperatureThe resulting gummy mass was heated
  2. temperatureto reflux
  3. temperaturemaintained for 15 minutes
  4. filtrationThe precipitated product was collected by filtration
  5. washwashed with isopropyl alcohol (25 ml)
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-4d4e834c097e48cd99a19b42b4acf138
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08101597B2

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