反应 #586138

ord-bdf37e3e16564c87b53fee5c8ff3ae0c

反应方程式

Cc1ccc(-c2c[nH]nc2C(F)(F)F)cc1SCC(F)(F)F
[2-methyl-5-(3-trifluoromethylpyrazolyl)phenyl] 2,2,2-trifluoroethyl sulfide
O=S([O-])[O-].[Na+].[Na+]
sodium sulfite
Cc1ccc(-c2c[nH]nc2C(F)(F)F)cc1S(=O)CC(F)(F)F
[2-methyl-5-(3-trifluoromethylpyrazolyl)phenyl] 2,2,2-trifluoroethyl sulfoxide
收率 37.1%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGthe reaction mixture was stirred at 0° C. 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 1.68 g (4.9 mmol) of [2-methyl-5-(3-trifluoromethylpyrazolyl)phenyl] 2,2,2-trifluoroethyl sulfide (Compound No. V-292 of the present invention) in 5 ml of chloroform, 1.02 g (5.1 mmol) of m-chlotoperbenzoic acid was added at 0° C. with stirring, and the reaction mixture was stirred at 0° C. 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 0.65 g of [2-methyl-5-(3-trifluoromethylpyrazolyl)phenyl] 2,2,2-trifluoroethyl sulfoxide (yield 37.1%) as a pale yellow solid (m.p. 109-110° C.).

来源

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