HRID1625683

反应详情

EQUATION

反应方程式

HRID 1625683 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 30 wt % aqueous solution of hydrogen peroxide (50 μL) was added to a trifluoroacetic acid solution of 3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-5-fluoromethyl-4-trifluoromethylthiopyrazole (205 mg) prepared as described in Example 30. The reaction mixture was stirred for 6 h whereupon solvent was evaporated under reduced pressure to give a residue that was purified by chromatography (SiO2, heptane/DCM) to afford the title compound as a white solid (66.5 mg, 32%). MS (ES): M/Z [M−H] 452. 1H NMR: (400 MHz, DMSO-d6): 5.48-5.75 (m, 2H) and 8.41 (s, 2H). 19F NMR (376 MHz, DMSO-d6): −62.05 (s, 3F), −73.68 (d, 3F) and −82.41 (m, 1F).

WORKUP

后处理

  1. customprepared
  2. customwas evaporated under reduced pressure
  3. customto give a residue that
  4. customwas purified by chromatography (SiO2, heptane/DCM)