反应 #1880954

反应方程式

water

NaH

4-trifluoromethylpyrazole

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

→

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

收率 14.9%

溶剂

dimethylacetamide

反应条件

后处理

1. 1
   温度cooled to RT
2. 2
   萃取After threefold extraction with ethyl acetate the product
3. 3
   洗涤is washed with water and saturated sodium chloride solution
4. 4
   干燥dried over MgSO4
5. 5
   浓缩concentrated
6. 6
   其他Chromatographic purification on silica gel with heptane/ethyl acetate (3:7) as eluent

实验过程

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.

来源