反応 #2348089

反応方程式

hydrogen peroxide

compound ( 3 )

2,3-difluoro-5-methylphenylboric acid

→

2,3-difluoro-5-methylphenol

溶媒

sodium hydrogensulfite

反応条件

後処理

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

実験手順

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).

出典