Maltol → Gallium Maltol

HRID 1288800

Reaktionsgleichung

Reaktionsgleichung von HRID 1288800
[CH3:1][C:2]1[O:8][CH:7]=[CH:6][C:4](=[O:5])[C:3]=1[OH:9].[N+]([O-])([O-])=O.[Ga+3:14].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.C([O-])([O-])=O.[Na+].[Na+]>O>[Ga:14].[CH3:1][C:2]1[O:8][CH:7]=[CH:6][C:4](=[O:5])[C:3]=1[OH:9]

Komponenten

5

Edukt 3

HCID 8369MaltolHCID 10340Sodium Carbonate2×HCID 61635Gallium nitrate

Produkt 1

HCID 10198059Gallium Maltol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
23 °C

Versuchsvorschrift

Maltol is dissolved in chloroform to form a 0.75M solution, and gallium nitrate nonohydrate is dissolved in ethanol to form a 0.5M solution. To 20 mL of the 0.75M maltol solution is slowly added, with continuous stirring, 10 mL of the 0.5M gallium nitrate nonohydrate solution. The resulting solution is stirred for 5 minutes at 23° C. Approximately 5.5 g (a large excess) of powdered Na2CO3 is added with stirring to raise the pH to close to 7. When the sodium carbonate is added, a trace of water may sometimes need to be added to facilitate the reaction, which is evidenced by some effervescence. Stirring is then continued for an additional ten minutes. The mixture is filtered to remove all solids, and the filtrate is evaporated in a rotary evaporator. The remaining crystalline solid is the 3:1 maltol:gallium composition. This composition is analyzed using powder x-ray diffraction and found to consist of orthothrombic crystals with unit cell dimensions of about a=18.53(1)Å, b=16.96(1)Å, c=12.05(1)Å. Crystallization from other solvents or under other conditions may produce other crystal structures. It is contemplated that amorphous structures can also be used in the methods and compositions of this invention.

Aufarbeitung

  1. stirringwith stirring
  2. temperatureto raise the pH
  3. customto close to 7
  4. additionto be added
  5. customthe reaction, which
  6. stirringStirring
  7. waitis then continued for an additional ten minutes
  8. filtrationThe mixture is filtered
  9. customto remove all solids
  10. customthe filtrate is evaporated in a rotary evaporator
  11. customCrystallization from other solvents
  12. customunder other conditions may produce other crystal structures

Quellen und Nachweise

ORD-Eintrag
ord-1c0bea6fd21a45b6be3792c5ce70455e
Quelldatensatz
uspto-grants-1998_05
Patentnummer
US05747482

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