반응 #51597

반응 방정식

2,4,6-trifluoropyridine

5-hydroxy-1-methyl-3-trifluoromethylpyrazole

potassium carbonate

→

colorless crystals

수율 93.0%

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

수율 93.0%

용매

sulfolane

pentane ethyl acetate

isopropyl ether

반응 조건

후처리

1. 1
   온도After cooling
2. 2
   여과filtered through a bed of silica gel
3. 3
   세척The filtrate is washed 10 times with water
4. 4
   건조the organic layer is dried over magnesium sulfate
5. 5
   기타After removal of the solvents

실험 절차

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.

출처