HRID1383600

反应详情

EQUATION

反应方程式

HRID 1383600 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Isopropyltriphenylphosphonium iodide (0.97 g) in anhydrous ether (10 ml) was treated at room temperature with n-butyllithium (0.9 ml of a 2.5M solution in hexanes). To the resulting dark red solution was added 3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)4-formylpyrazole (0.6 g) in ether (20 ml) and the mixture stirred for 2 hours. The solution was washed with water (20 ml) and the separated organic layer dried (MgSO4) and evaporated. The residue was purified by column chromatography on silica gel eluted with dichloromethane. Combination and evaporation of suitable fractions provided the title compound as a pale tan solid m.p. 72-74° C.

WORKUP

后处理

  1. washThe solution was washed with water (20 ml)
  2. dry with materialthe separated organic layer dried (MgSO4)
  3. customevaporated
  4. customThe residue was purified by column chromatography on silica gel
  5. washeluted with dichloromethane
  6. customCombination and evaporation of suitable fractions