반응 #2348098

반응 방정식

compound ( 10 )

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

hydrogen peroxide

sodium

→

2,3-difluoro-5-methylphenol

용매

THF

반응 조건

후처리

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

실험 절차

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 hydrogensufite 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).

출처