HRID1383613
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe reaction mixture was evaporated
- washwashed with water
- customThe organic layer was separated
- customdried
- customevaporated
- customThe residue was purified by column chromatography on silica gel (10 g)
- washeluted with hexane
- customCombination and evaporation of appropriate fractions