Reacción #53575

Ecuación de reacción

2-(2,2,2-trifluoroethylthio)-4-(3-trifluoromethylpyrazolyl)benzaldehyde

dioxane

potassium carbonate

→

[2-ethenyl-5-(3-trifluoromethylpyrazolyl)phenyl] 2,2,2-trifluoroethyl sulfide

Rendimiento 43.8%

Disolventes

water

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturawith heating for 5 hours
2. 2
   Filtraciónthe insolubles were filtered off
3. 3
   workup.DISTILLATIONthe dioxane was distilled off under reduced pressure
4. 4
   OtroPurification of the residue by silica gel column chromatography

Procedimiento

2.83 g (8.0 mmol) of 2-(2,2,2-trifluoroethylthio)-4-(3-trifluoromethylpyrazolyl)benzaldehyde (Compound No. V-275 of the present invention) prepared in the same manner as in Example 8 (9), 2.85 g (8.0 mmol) of methyltriphenylphosphonium bromide and 1.38 g (10.0 mmol) of potassium carbonate were refluxed in a solvent mixture of 20 ml of dioxane and 0.3 ml of water with heating for 5 hours. After cooling down to room temperature, the insolubles were filtered off, and the dioxane was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 1.23 g of [2-ethenyl-5-(3-trifluoromethylpyrazolyl)phenyl] 2,2,2-trifluoroethyl sulfide (yield 43.8%) as a pale yellow liquid (nD20 1.5328).

Fuente