Oxalic acid dihydrate → Escitalopram Oxalate

HRID 1174049

Reaktionsgleichung

Reaktionsgleichung von HRID 1174049
O.O.[C:3]([OH:8])(=[O:7])[C:4]([OH:6])=[O:5].[CH3:9][N:10]([CH2:12][CH2:13][CH2:14][C@@:15]1([C:26]2[CH:27]=[CH:28][C:29]([F:32])=[CH:30][CH:31]=2)[O:23][CH2:22][C:21]2[CH:20]=[C:19]([C:24]#[N:25])[CH:18]=[CH:17][C:16]1=2)[CH3:11]>CC(O)C>[CH3:9][N:10]([CH2:12][CH2:13][CH2:14][C@@:15]1([C:26]2[CH:31]=[CH:30][C:29]([F:32])=[CH:28][CH:27]=2)[O:23][CH2:22][C:21]2[CH:20]=[C:19]([C:24]#[N:25])[CH:18]=[CH:17][C:16]1=2)[CH3:11].[C:4]([OH:6])([C:3]([OH:8])=[O:7])=[O:5]

Komponenten

4

Edukt 2

HCID 61373Oxalic acid dihydrateHCID 146570Escitalopram

Produkt 1

HCID 146571Escitalopram Oxalate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel2×

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

100 g of the free base was dissolved in 250 mL of 2-propanol. 1 eq. of oxalic acid dihydrate was dissolved in 250 mL of warm 2-propanol and was added at 40° C. to the solution of escitalopram base. After stirring at 40° C. for 10 min the crystallization started. The mixture was then allowed to cool to room temperature and stirred for ca. 2 hours. The crystals were filtered off, rinsed on the filter with 2-propanol and dried to constant weight under vacuum at 60° C.

Aufarbeitung

  1. customthe crystallization
  2. temperatureto cool to room temperature
  3. stirringstirred for ca. 2 hours
  4. filtrationThe crystals were filtered off
  5. washrinsed on the
  6. filtrationfilter with 2-propanol
  7. customdried to constant weight under vacuum at 60° C.

Quellen und Nachweise

ORD-Eintrag
ord-2f5dc779cec14e3fb4083b9544b5a79c
Quelldatensatz
uspto-grants-2010_11
Patentnummer
US07834201B2

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