Reaktion #1100084

Reaktionsgleichung

hydrogen peroxide

compound ( 10 )

2,3-difluoro-4-ethoxy-6-methylphenylboric acid

sodium hydrogen sulfite

→

2,3-difluoro-5-methylphenol

Lösungsmittel

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturUnder cooling with an ice bath
2. 2
   TemperaturUnder cooling with an ice bath
3. 3
   Sonstigeto terminate
4. 4
   Sonstigethe reaction
5. 5
   Extraktionan aqueous layer was extracted with diethyl ether, which
6. 6
   workup.ADDITIONwas added to the organic layer
7. 7
   WaschenThe organic layer was washed with a saturated sodium hydrogensufite aqueous solution and saturated saline
8. 8
   Trocknendried over anhydrous magnesium sulfate
9. 9
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure

Vorschrift

Under cooling with an ice bath, 6.57 g of aqueous hydrogen peroxide was slowly added dropwise to the compound (10) having been dissolved in 37 mL of THF, followed by stirring at room temperature for 3 hours. Under cooling with an ice bath, 20 mL of a saturated sodium hydrogen sulfite aqueous solution was added thereto to terminate the reaction, and an aqueous layer was extracted with diethyl ether, which was added to the organic layer. The organic layer was washed with a saturated sodium hydrogensufite aqueous solution and saturated saline, and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 3.84 g of 2,3-difluoro-5-methylphenol (11).

Quelle