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Oxalic Acid → Oxcarbazepine

HRID 41348
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 41348
C[O:2][C:3]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[N:11]([C:18]([NH2:20])=[O:19])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=1.C(O)(=O)C(O)=O.C(O)(C)C>O>[CH:7]1[CH:8]=[CH:9][C:10]2[N:11]([C:18]([NH2:20])=[O:19])[C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][C:17]=3[C:3](=[O:2])[CH2:4][C:5]=2[CH:6]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 971Oxalic AcidHCID 3776IsopropanolHCID 12003110-methoxy-5H-dibenz(b,f)azepine-5-carboxamide

Produkt 1

HCID 34312OxcarbazepineAusbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

100 g of 10-methoxycarbamazepine in 1000 ml water and 69.24 g of oxalic acid solution were heated to 90° C. and maintained for about 17 hrs. After completion of the reaction the reaction mixture was cooled to room temperature (RT). The resulting reaction mass was filtered and washed with 1000 ml of DM water. The wet material obtained was charged with isopropyl alcohol and DM water. The obtained reaction mixture was heated to reflux for about 2 h. The reaction mixture was cooled to 15-25° C., filtered and washed with 100 ml of IPA-water mixture. The resulting compound is dried at 60° C. for 6 h to produce 90 g of Oxcarbazepine.

Aufarbeitung

  1. temperaturemaintained for about 17 hrs
  2. customAfter completion of the reaction the reaction mixture
  3. customThe resulting reaction mass
  4. filtrationwas filtered
  5. washwashed with 1000 ml of DM water
  6. customThe wet material obtained
  7. customThe obtained reaction mixture
  8. temperaturewas heated
  9. temperatureto reflux for about 2 h
  10. temperatureThe reaction mixture was cooled to 15-25° C.
  11. filtrationfiltered
  12. washwashed with 100 ml of IPA-water mixture
  13. customThe resulting compound is dried at 60° C. for 6 h

Quellen und Nachweise

ORD-Eintrag
ord-585b8bb396a54b5a902a8c118e5880f7
Quelldatensatz
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08530647B2

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