Water → HCID 14304992, Verbindung

HRID 2050683Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2050683
C[O:2][C:3]1[CH:4]=[C:5]([CH:20]=[C:21]([O:25]C)[C:22]=1[O:23]C)[C:6]1[O:7][C:8]2[C:13]([C:14](=[O:19])[C:15]=1[C:16]([OH:18])=[O:17])=[CH:12][CH:11]=[CH:10][CH:9]=2.B(Br)(Br)Br.O>ClCCl>[OH:25][C:21]1[CH:20]=[C:5]([CH:4]=[C:3]([OH:2])[C:22]=1[OH:23])[C:6]1[O:7][C:8]2[C:13]([C:14](=[O:19])[C:15]=1[C:16]([OH:18])=[O:17])=[CH:12][CH:11]=[CH:10][CH:9]=2

Komponenten

5

Edukt 3

HCID 962Water2×HCID 25134Boron tribromideHCID 143049774-Oxo-2-(3,4,5-trimethoxyphenyl)-4H-1-benzopyran-3-carboxylic acid

Produkt 1

HCID 14304992HCID 14304992, VerbindungAusbeute 85 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

4.0 g of 3',4',5'-trimethoxyflavone-3-carboxylic acid were added to 200 ml of absolute dichloromethane and reacted with 82 ml of a 1 molar boron tribromide solution in absolute dichloromethane under a nitrogen atmosphere at 0° C. The reaction mixture was stirred for twelve hours during which it was allowed to warm to room temperature. Then, for working up, water was carefully added under ice cooling, then made up to twice the volume with water and intensively stirred. The resulting 3',4',5'-trihydroxyflavone-3-carboxylic acid precipitated and was filtered out. The filter cake was washed with water several times and recrystallized from methanol. 3 g of pure 3',4',5'-trihydroxyflavone-3-carboxylic acid were obtained.

Aufarbeitung

  1. stirringintensively stirred
  2. customThe resulting 3',4',5'-trihydroxyflavone-3-carboxylic acid precipitated
  3. filtrationwas filtered out
  4. washThe filter cake was washed with water several times
  5. customrecrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-26024188fb0b42ddb58631608b83297b
Quelldatensatz
uspto-grants-1991_05
Patentnummer
US05013852

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