Reaktion #95369

Reaktionsgleichung

sodium chlorite

sulfamic acid

( 2 )

6,7-Bis(ethoxycarbonyloxy)chromone-3-carboxaldehyde

→

desired product

6,7-Bis(ethoxycarbonyloxy)chromone-3-carboxylic acid

Lösungsmittel

water

water

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGThe solution was stirred at the same temperature for 1 hour
2. 2
   Sonstigeto separate
3. 3
   WaschenThe dichloromethane layer was washed with water (once) and then with a saturated aqueous solution of sodium chloride (twice), and
4. 4
   Trocknendried over magnesium sulfate
5. 5
   workup.DISTILLATIONThe solvent was distilled off
6. 6
   workup.ADDITIONethyl ether was added to the residue
7. 7
   Sonstigeto triturate it
8. 8
   FiltrationThe triturated product was collected by filtration
9. 9
   Sonstigedried

Vorschrift

The compound (1.05 g) obtained in (2) was dissolved in of dichloromethane (31.5 ml) and a solution of 1.05 g of sulfamic acid in water (18.9 ml) was added at 10° C. with stirring. Then, a solution of sodium chlorite (525.6 mg) in water (1.2 ml) was added. The solution was stirred at the same temperature for 1 hour, and allowed to separate. The dichloromethane layer was washed with water (once) and then with a saturated aqueous solution of sodium chloride (twice), and dried over magnesium sulfate. The solvent was distilled off, and ethyl ether was added to the residue to triturate it. The triturated product was collected by filtration, and dried to afford the desired product (950 mg).

Quelle