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Barium hydroxide, octahydrate → HCID 131733076, Verbindung

HRID 2201654
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2201654
[OH2:1].[NH2:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10](=[O:16])/[CH:11]=[CH:12]\[C:13]([OH:15])=[O:14])=[CH:5][CH:4]=1.O.O.O.O.O.O.O.O.[OH-].[Ba+2:26].[OH-]>O>[OH2:14].[OH2:1].[NH2:2][C:3]1[CH:4]=[CH:5][C:6]([NH:9][C:10](=[O:16])/[CH:11]=[CH:12]\[C:13]([O-:15])=[O:14])=[CH:7][CH:8]=1.[NH2:2][C:3]1[CH:4]=[CH:5][C:6]([NH:9][C:10](=[O:16])/[CH:11]=[CH:12]\[C:13]([O-:15])=[O:14])=[CH:7][CH:8]=1.[Ba+2:26]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 17749109Barium hydroxide, octahydrateHCID 86708816HCID 86708816, Verbindung

Produkt 1

HCID 131733076HCID 131733076, VerbindungAusbeute 142,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

Under a nitrogen atmosphere, into a reaction vessel were charged 10.0 g (44.6 mmol) of (2Z)-4-[(4-aminophenyl)amino]-4-oxo-2-butenoic acid mono-hydrate obtained by the same method as in Production Example 2 and 70 ml of water, a solution prepared by dissolving 7.04 g (22.3 mmol) of barium hydroxide octa-hydrate in 30 ml of water was added at 20 to 30° C., and the mixture was stirred at room temperature for 2 hours. Thereafter, the mixture was condensed under reduced pressure and the solvent was distilled off to obtain a residue to which 50 ml of ethanol and 50 ml of 2-propanol were added, and the mixture was stirred at room temperature overnight, the deposited crystal was isolated by filtration, and dried under reduced pressure at 45° C., to obtain 12.4 g of barium bis{(2Z)-4-[(4-aminophenyl)amino]-4-oxo-2-butenoate}di-hydrate as a yellow solid. Yield: 98.3%.

Aufarbeitung

  1. customa solution prepared
  2. additionwas added at 20 to 30° C.
  3. customcondensed under reduced pressure
  4. distillationthe solvent was distilled off
  5. customto obtain a residue to which 50 ml of ethanol and 50 ml of 2-propanol
  6. additionwere added
  7. stirringthe mixture was stirred at room temperature overnight
  8. customthe deposited crystal was isolated by filtration
  9. customdried under reduced pressure at 45° C.

Quellen und Nachweise

ORD-Eintrag
ord-4ffc4385f9ab46c9976aaa9a09f905bd
Quelldatensatz
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09365497B2

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