反应 #1876814
ord-f03a97a4a3344ae59edc0baf9053a4fa
反应方程式
sodium hydrogen sulfite
hydrogen peroxide water
Acetic acid
Compound ( d )
4-ethoxy-2-trifluoromethylphenylboric Acid
→
Compound ( e )
收率 97.7%
4-ethoxy-2-trifluoromethylphenol
收率 97.7%
反应物
试剂
无
溶剂
反应条件
温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他the resulting reaction mixture
- 2温度was carefully heated
- 3workup.STIRRINGstirred at 50° C. for 4 hours
- 4萃取the reaction mixture was extracted three times with ether
- 5洗涤washed with aqueous saturated sodium hydrogen sulfite
- 6干燥dried over anhydrous magnesium sulfate
- 7workup.DISTILLATIONThe solvent was distilled off under reduced pressure
实验过程
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).