Methanol → 5,7-Dihydroxy-2-methylsulfinylchromone

HRID 441055Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 441055
OO[S:3]([O-:5])=O.[K+].[OH:7][C:8]1[CH:17]=[C:16]([OH:18])[CH:15]=[C:14]2[C:9]=1[C:10](=S)[CH:11]=[C:12](C)[O:13]2.[OH2:21].[CH3:22]O>>[OH:7][C:8]1[CH:17]=[C:16]([OH:18])[CH:15]=[C:14]2[C:9]=1[C:10](=[O:21])[CH:11]=[C:12]([S:3]([CH3:22])=[O:5])[O:13]2

Komponenten

5

Edukt 4

HCID 887MethanolHCID 962WaterHCID 23707502Potassium hydroxy sulfiteHCID 1361024115,7-Dihydroxy-2-methylthiochromone

Produkt 1

HCID 229064885,7-Dihydroxy-2-methylsulfinylchromone

Versuchsvorschrift

1 ml aqueous solution of 82 mg oxone (0.134 mmol) was added dropwise to 1 ml of 30 mg of 5,7-dihydroxy-2-methylthiochromone (0.134 mmol) in methanol at room temperature, and the mixture was stirred for 1 hour. After addition of water, the reaction solution was extracted twice with ethyl acetate, and the organic layer was washed with saturated NaCl water and dried over sodium sulfate anhydride. The solvent was distilled off under reduced pressure, to give 32 mg of 5,7-dihydroxy-2-methylsulfinylchromone (containing a little sulfone). This product was subjected without purification to the following reaction.

Aufarbeitung

  1. extractionthe reaction solution was extracted twice with ethyl acetate
  2. washthe organic layer was washed with saturated NaCl water
  3. dry with materialdried over sodium sulfate anhydride
  4. distillationThe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-88cbf3a340834ba8afc8d06bfd0a69fa
Quelldatensatz
uspto-grants-1996_05
Patentnummer
US05521216

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