Maltol → Gallium Maltol

HRID 1288800ノート

反応式

HRID 1288800 の反応式
[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]

参加物

5

反応物 3

HCID 8369MaltolHCID 10340Sodium Carbonate2 回HCID 61635Gallium nitrate

生成物 1

HCID 10198059Gallium Maltol

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
23 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1c0bea6fd21a45b6be3792c5ce70455e
出典データセット
uspto-grants-1998_05
特許番号
US05747482

反応ノート

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