Maleic Acid → 5-chloro-2-methyl-2,3,3a,12b-tetrahydro-1H-dibenzo[2,3:6,7]oxepino[4,5-c]pyrrole maleate

HRID 63782

Reaktionsgleichung

[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]\[C:4]([OH:6])=[O:5].[CH3:9][N:10]1[CH2:27][CH:26]2[CH:12]([C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=3[O:19][C:20]3[CH:21]=[CH:22][C:23]([Cl:28])=[CH:24][C:25]=32)[CH2:11]1>C(O)(C)C>[CH3:9][N:10]1[CH2:27][CH:26]2[CH:12]([C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=3[O:19][C:20]3[CH:21]=[CH:22][C:23]([Cl:28])=[CH:24][C:25]=32)[CH2:11]1.[CH:2](/[C:1]([OH:8])=[O:7])=[CH:3]/[C:4]([OH:6])=[O:5]

Komponenten

Reaktionsbedingungen

Temperatur: 50 °C

Versuchsvorschrift

1.38 Kg of asenapine phosphate is loaded into a reactor. Toluene (15 L) is added, and the suspension is placed under stirring. A 9% solution of sodium bicarbonate (15 L) is added by dripping. The solution is left under stirring at 25° C. for 30 minutes. The lower aqueous phase is eliminated. The organic phase is washed with water (2×7 L). The solvent is evaporated under vacuum, obtaining asenapine base (0.90 Kg) in the form of oil. Isopropanol (12 L) is loaded into the reactor and dissolved by heating at 50° C. Maleic acid (0.4 Kg) is added to the asenapine base solution at 50° C. The solution is cooled to 25° C. in approx. 2 hours. The solution is left under stirring at 25° C. for 2 hours. The product is isolated by filtration, washing with isopropanol (3 L). The product is dried under vacuum at 50° C. for 20 hours. 1 Kg of asenapine maleate is obtained.

Aufarbeitung

dissolutiondissolved
temperatureThe solution is cooled to 25° C. in approx. 2 hours
waitThe solution is left
customThe product is isolated by filtration
washwashing with isopropanol (3 L)
customThe product is dried under vacuum at 50° C. for 20 hours

Quellen und Nachweise

ORD-Eintrag: ord-ddbe03bdd2664907a304af5ad5833a84
Quelldatensatz: uspto-grants-2016_09
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US09447109B2

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