반응 #2348089

반응 방정식

hydrogen peroxide

compound ( 3 )

2,3-difluoro-5-methylphenylboric acid

→

2,3-difluoro-5-methylphenol

용매

sodium hydrogensulfite

반응 조건

후처리

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

실험 절차

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).

출처