反应 #1876814

ord-f03a97a4a3344ae59edc0baf9053a4fa

反应方程式

O=S([O-])O.[Na+]
sodium hydrogen sulfite
O.OO
hydrogen peroxide water
CC(=O)O
Acetic acid
CCOc1ccc(OB(O)O)c(C(F)(F)F)c1
Compound ( d )
CCOc1ccc(OB(O)O)c(C(F)(F)F)c1
4-ethoxy-2-trifluoromethylphenylboric Acid
CCOc1ccc(O)c(C(F)(F)F)c1
Compound ( e )
收率 97.7%
CCOc1ccc(O)c(C(F)(F)F)c1
4-ethoxy-2-trifluoromethylphenol
收率 97.7%

溶剂

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他the resulting reaction mixture
  2. 2
    温度was carefully heated
  3. 3
    workup.STIRRINGstirred at 50° C. for 4 hours
  4. 4
    萃取the reaction mixture was extracted three times with ether
  5. 5
    洗涤washed with aqueous saturated sodium hydrogen sulfite
  6. 6
    干燥dried over anhydrous magnesium sulfate
  7. 7
    workup.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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07070838B2uspto-grants-2006_07