Dimethylformamide → HCID 58913661, Verbindung

HRID 1296951Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1296951
[Cl:1][C:2]1[C:3]([OH:21])=[C:4]([CH3:20])[C:5]([OH:19])=[C:6]([C:8](=[O:18])[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=2)[CH:7]=1.CN(C=O)C.C([O-])([O-])=O.[K+].[K+].[C:33](OC(=O)C)(=O)[CH3:34]>O>[Cl:1][C:2]1[CH:7]=[C:6]2[C:5](=[C:4]([CH3:20])[C:3]=1[OH:21])[O:19][C:33]([CH3:34])=[C:9]([C:10]1[CH:11]=[CH:12][C:13]([O:16][CH3:17])=[CH:14][CH:15]=1)[CH:8]2[OH:18]

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 7918Acetic AnhydrideHCID 11430Potassium CarbonateHCID 58913540HCID 58913540, Verbindung

Produkt 1

HCID 58913661HCID 58913661, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution of 1-(5-chloro-2,4-dihydroxy-3-methyl-phenyl)-2-(4-methoxy-phenyl)-ethanone (1 eq) in an. DMF (7 ml) was added K2CO3 (3 eq). Acetic anhydride (3 eq) was added dropwise to the solution, which was then refluxed under nitrogen whilst stirring for 5 h. The solution was taken up in water and extracted using ethyl acetate, dried over MgSO4 and concentrated in vacuo to give 6-chloro-3-(4-methoxy-phenyl)-2,8-dimethyl-4H-chromene-4,7-diol as a crystalline solid.

Aufarbeitung

  1. temperaturewas then refluxed under nitrogen
  2. extractionextracted
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-bf85aa3446604a58a04d70bd7402924b
Quelldatensatz
uspto-grants-2007_07
Patentnummer
US07247734B2

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