تفاعل #1880954

معادلة التفاعل

water

NaH

4-trifluoromethylpyrazole

2-fluoro-6-(2-trifluormethyl-4-thienyloxy)pyridine

→

2-(4-trifluoromethylpyrazol-1-yl)-6-(2-trifluoromethyl-4-thienyloxy)pyridine

المردود 14.9%

المذيبات

dimethylacetamide

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooled to RT
2. 2
   استخلاصAfter threefold extraction with ethyl acetate the product
3. 3
   غسيلis washed with water and saturated sodium chloride solution
4. 4
   تجفيفdried over MgSO4
5. 5
   تركيزconcentrated
6. 6
   أخرىChromatographic purification on silica gel with heptane/ethyl acetate (3:7) as eluent

الإجراء التجريبي

0.114 g of 4-trifluoromethylpyrazole is introduced in 5 ml of dimethylacetamide under nitrogen and at 0° C. 0.028 g of NaH is added. The mixture is allowed to come to RT over 30 min and then 0.2 g of 2-fluoro-6-(2-trifluormethyl-4-thienyloxy)pyridine is added and the mixture is heated at 80° C. for 9 h, cooled to RT and poured into water. After threefold extraction with ethyl acetate the product is washed with water and saturated sodium chloride solution, dried over MgSO4 and concentrated. Chromatographic purification on silica gel with heptane/ethyl acetate (3:7) as eluent gives 0.043 g of 2-(4-trifluoromethylpyrazol-1-yl)-6-(2-trifluoromethyl-4-thienyloxy)pyridine as colorless crystals.

المصدر