تفاعل #51597

معادلة التفاعل

2,4,6-trifluoropyridine

5-hydroxy-1-methyl-3-trifluoromethylpyrazole

potassium carbonate

→

colorless crystals

المردود 93.0%

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

المردود 93.0%

المذيبات

sulfolane

pentane ethyl acetate

isopropyl ether

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling
2. 2
   ترشيحfiltered through a bed of silica gel
3. 3
   غسيلThe filtrate is washed 10 times with water
4. 4
   تجفيفthe organic layer is dried over magnesium sulfate
5. 5
   أخرىAfter removal of the solvents

الإجراء التجريبي

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.

المصدر