반응 #1876814

반응 방정식

sodium hydrogen sulfite

hydrogen peroxide water

Acetic acid

Compound ( d )

4-ethoxy-2-trifluoromethylphenylboric Acid

→

Compound ( e )

수율 97.7%

4-ethoxy-2-trifluoromethylphenol

수율 97.7%

용매

THF

반응 조건

후처리

1. 1
   기타the resulting reaction mixture
2. 2
   온도was carefully heated
3. 3
   workup.STIRRINGstirred at 50° C. for 4 hours
4. 4
   추출the reaction mixture was extracted three times with ether
5. 5
   세척washed with aqueous saturated sodium hydrogen sulfite
6. 6
   건조dried over anhydrous magnesium sulfate
7. 7
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure

실험 절차

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).

출처