反应 #586137

ord-a1db2cdff5bd4d6f87977ad6496ee5ab

反应方程式

O=C(OO)c1cccc(Cl)c1
m-chloroperbenzoic acid
FC(F)c1ccc(-c2c[nH]nc2C(F)(F)F)cc1SCC(F)(F)F
[2-difluoromethyl-5-(3-trifluoromethylpyrazolyl)phenyl] 2,2,2-trifluoroethyl sulfide
O=S([O-])[O-].[Na+].[Na+]
sodium sulfite
O=S(CC(F)(F)F)c1cc(-c2c[nH]nc2C(F)(F)F)ccc1C(F)F
[2-difluoromethyl-5-(3-trifluoromethylpyrazolyl)phenyl] 2,2,2-trifluoroethyl sulfoxide
收率 97.4%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGthe reaction solution was stirred for 1 hour
  2. 2
    workup.STIRRINGstirred at room temperature for 10 minutes
  3. 3
    洗涤The chloroform layer was washed with 20 ml of saturated aqueous sodium hydrogen carbonate three times
  4. 4
    干燥dried over anhydrous magnesium sulfate
  5. 5
    workup.DISTILLATIONthe chloroform was distilled off under reduced pressure

实验过程

To 0.37 g (1.0 mmol) of [2-difluoromethyl-5-(3-trifluoromethylpyrazolyl)phenyl] 2,2,2-trifluoroethyl sulfide (Compound No. V-295 of the present invention) in 5 ml of chloroform, 0.25 g (1.5 mmol) of m-chloroperbenzoic acid was added at 0° C. with stirring, and the reaction solution was stirred for 1 hour. The reaction solution was mixed with 10 ml of 10% aqueous sodium sulfite and stirred at room temperature for 10 minutes, and then 20 ml of chloroform was added. The chloroform layer was washed with 20 ml of saturated aqueous sodium hydrogen carbonate three times and dried over anhydrous magnesium sulfate, and the chloroform was distilled off under reduced pressure to obtain 0.38 g of [2-difluoromethyl-5-(3-trifluoromethylpyrazolyl)phenyl] 2,2,2-trifluoroethyl sulfoxide (yield 97.4%) as a yellow dough (nD2 1.4909).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07767626B2uspto-grants-2010_08