HRID1383613

反应详情

EQUATION

反应方程式

HRID 1383613 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of 1-(2,6-dichloro-4-trifluoromethylphenyl)4-ethynyl-3-methylpyrazole (0.53 g) in acetone (5 ml) was added N-bromosuccinimide (0.295 g) and silver nitrate (0.028 g). Stirring was continued at room temperature for 1 hour. The reaction mixture was evaporated and the residue taken up in ether and washed with water. The organic layer was separated, dried and evaporated. The residue was purified by column chromatography on silica gel (10 g) eluted with hexane and then dichioromethane: hexane (1:1). Combination and evaporation of appropriate fractions, followed by crystailisation from hexane, gave the title compound as a very pale yellow solid m.p. 86-89° C.

WORKUP

后处理

  1. customThe reaction mixture was evaporated
  2. washwashed with water
  3. customThe organic layer was separated
  4. customdried
  5. customevaporated
  6. customThe residue was purified by column chromatography on silica gel (10 g)
  7. washeluted with hexane
  8. customCombination and evaporation of appropriate fractions