Reacción #51597

Ecuación de reacción

2,4,6-trifluoropyridine

5-hydroxy-1-methyl-3-trifluoromethylpyrazole

potassium carbonate

→

colorless crystals

Rendimiento 93.0%

2,4,6-Tris(1-methyl-3-trifluoromethylpyrazol-5-yloxy)pyridine

Rendimiento 93.0%

Disolventes

sulfolane

pentane ethyl acetate

isopropyl ether

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaAfter cooling
2. 2
   Filtraciónfiltered through a bed of silica gel
3. 3
   LavadoThe filtrate is washed 10 times with water
4. 4
   Secadothe organic layer is dried over magnesium sulfate
5. 5
   OtroAfter removal of the solvents

Procedimiento

A mixture of 4.8 g (36 mmol) 2,4,6-trifluoropyridine, 19.8 g (119 mmol) 5-hydroxy-1-methyl-3-trifluoromethylpyrazole and 18.1 g (131 mmol) potassium carbonate in 25 ml anhydrous sulfolane is stirred and heated to 80° C. over a period of 3 days. After cooling, the mixture is diluted with pentane/ethyl acetate (by volume ration 1/1) and filtered through a bed of silica gel. The filtrate is washed 10 times with water and the organic layer is dried over magnesium sulfate. After removal of the solvents, the residue is washed with isopropyl ether and 19.1 g (93% yield) colorless crystals of melting point 130° C. are obtained.

Fuente