HRID1348995

反应详情

EQUATION

反应方程式

HRID 1348995 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

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.

WORKUP

后处理

  1. temperaturecooled to RT
  2. extractionAfter threefold extraction with ethyl acetate the product
  3. washis washed with water and saturated sodium chloride solution
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. customChromatographic purification on silica gel with heptane/ethyl acetate (3:7) as eluent