反応 #2348098

反応方程式

compound ( 10 )

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

hydrogen peroxide

sodium

→

2,3-difluoro-5-methylphenol

溶媒

THF

反応条件

後処理

1. 1
   温度Under cooling with an ice bath
2. 2
   温度Under cooling with an ice bath
3. 3
   その他to terminate
4. 4
   その他the reaction
5. 5
   抽出an aqueous layer was extracted with diethyl ether, which
6. 6
   workup.ADDITIONwas added to the organic layer
7. 7
   洗浄The organic layer was washed with a saturated sodium hydrogensufite aqueous solution and saturated saline
8. 8
   乾燥dried over anhydrous magnesium sulfate
9. 9
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure

実験手順

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).

出典