Реакция #51597

Уравнение реакции

2,4,6-trifluoropyridine

5-hydroxy-1-methyl-3-trifluoromethylpyrazole

potassium carbonate

→

colorless crystals

Выход 93.0%

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

Выход 93.0%

Растворители

sulfolane

pentane ethyl acetate

isopropyl ether

Условия реакции

Обработка

1. 1
   ТемператураAfter cooling
2. 2
   Фильтрацияfiltered through a bed of silica gel
3. 3
   ПромывкаThe filtrate is washed 10 times with water
4. 4
   Сушкаthe organic layer is dried over magnesium sulfate
5. 5
   ДругоеAfter removal of the solvents

Методика

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.

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