반응 #1880954

반응 방정식

water

NaH

4-trifluoromethylpyrazole

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

→

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

수율 14.9%

용매

dimethylacetamide

반응 조건

후처리

1. 1
   온도cooled to RT
2. 2
   추출After threefold extraction with ethyl acetate the product
3. 3
   세척is washed with water and saturated sodium chloride solution
4. 4
   건조dried over MgSO4
5. 5
   농축concentrated
6. 6
   기타Chromatographic purification on silica gel with heptane/ethyl acetate (3:7) as eluent

실험 절차

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.

출처