反応 #1876814

反応方程式

sodium hydrogen sulfite

hydrogen peroxide water

Acetic acid

Compound ( d )

4-ethoxy-2-trifluoromethylphenylboric Acid

→

Compound ( e )

収率 97.7%

4-ethoxy-2-trifluoromethylphenol

収率 97.7%

溶媒

THF

反応条件

後処理

1. 1
   その他the resulting reaction mixture
2. 2
   温度was carefully heated
3. 3
   workup.STIRRINGstirred at 50° C. for 4 hours
4. 4
   抽出the reaction mixture was extracted three times with ether
5. 5
   洗浄washed with aqueous saturated sodium hydrogen sulfite
6. 6
   乾燥dried over anhydrous magnesium sulfate
7. 7
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure

実験手順

Acetic acid (21.3 g) was added to a mixture of THF (200 mL) and Compound (d) (8.28 g) at room temperature, and the mixture was stirred at 0° C. under a nitrogen atmosphere. After adding 30% hydrogen peroxide water (40.1 g) dropwise, the resulting reaction mixture was carefully heated and stirred at 50° C. for 4 hours. Saturated aqueous sodium hydrogen sulfite (200 mL) was then slowly added dropwise at 0° C., and the reaction mixture was extracted three times with ether. The organic layers were combined, washed with aqueous saturated sodium hydrogen sulfite, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 6.67 g of Compound (e).

出典