Pyridine → HCID 22252930, compound

Participants

Reaction Steps

To the solution of 1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-4-trifluoromethylsulfenyl-5-hydroxypyrazole (7.00 g, 16.6 mmol) and pyridine (4.91 g, 62.1 mmol) in 1,2-dichloroethane at room temperature was added trimethylacetyl chloride (4.37 g, 36.2 mmol) dropwise. Ice bath was used to maintain the temperature of the reaction. After 20 hr at room temperature, the orgainc layer was washed with five times of aqueous KHS04 till the aqueous solution was at pH 1. The orgainc layer was then dried (Mg SO4) and concentrated to give a solid residue. Upon chromatographic purification via silica gel column of the solid residue, after trituration with pentane, a off white solid (2.403 g, 28.6% yield, 97.0% HPLC puriety) was provided as the desired product, m. p. 82-83 C.

Provenance & Evidence