Reaktion #1880954

Reaktionsgleichung

water

NaH

4-trifluoromethylpyrazole

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

→

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

Ausbeute 14.9%

Lösungsmittel

dimethylacetamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooled to RT
2. 2
   ExtraktionAfter threefold extraction with ethyl acetate the product
3. 3
   Waschenis washed with water and saturated sodium chloride solution
4. 4
   Trocknendried over MgSO4
5. 5
   Einengenconcentrated
6. 6
   SonstigeChromatographic purification on silica gel with heptane/ethyl acetate (3:7) as eluent

Vorschrift

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.

Quelle