Reaktion #2348089

Reaktionsgleichung

hydrogen peroxide

compound ( 3 )

2,3-difluoro-5-methylphenylboric acid

→

2,3-difluoro-5-methylphenol

Lösungsmittel

sodium hydrogensulfite

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturUnder cooling with an ice bath
2. 2
   workup.DISSOLUTIONhaving been dissolved in 300 mL
3. 3
   TemperaturUnder cooling with an ice bath
4. 4
   Sonstigeto terminate
5. 5
   Sonstigethe reaction
6. 6
   ExtraktionThe aqueous layer was extracted with diethyl ether, which
7. 7
   workup.ADDITIONwas added to the organic layer
8. 8
   Waschenthe organic layer was washed with a saturated sodium hydrogensulfite aqueous solution
9. 9
   Trocknena saturated saline and then dried over anhydrous magnesium sulfate
10. 10
    workup.DISTILLATIONThe solvent was distilled off in vacuo

Vorschrift

Under cooling with an ice bath, 53.1 g of aqueous hydrogen peroxide was slowly added dropwise to the compound (3) having been dissolved in 300 mL, followed by stirring at room temperature for 3 hours. Under cooling with an ice bath, 100 mL of a saturated sodium hydrogensulfite aqueous solution was added dropwise thereto to terminate the reaction. The aqueous layer was extracted with diethyl ether, which was added to the organic layer, and the organic layer was washed with a saturated sodium hydrogensulfite aqueous solution and a saturated saline and then dried over anhydrous magnesium sulfate. The solvent was distilled off in vacuo to obtain 22.7 g of 2,3-difluoro-5-methylphenol (4).

Quelle