HRID1274352
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 solution of 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-(furan-3-yl)pyrazole (0.095 g) in acetonitrile (6 ml) was added N-chlorosuccinimide (0.0345 g). The mixture was left at room temperature for 1.5 hours and then poured into ether (50 ml) and water (50 ml). The layers were separated and the aqueous phase extracted with a second portion of ether (50 ml). The combined organic layers were washed with water (25 ml), then dried (Na2SO4) and evaporated. The residue was purified by column chromatography on silica gel (10 g) eluted with dichloromethane. Combination and evaporation of suitable fractions gave the title compound as a white solid, m.p. 153° C.
WORKUP
后处理
- customThe layers were separated
- extractionthe aqueous phase extracted with a second portion of ether (50 ml)
- washThe combined organic layers were washed with water (25 ml)
- dry with materialdried (Na2SO4)
- customevaporated
- customThe residue was purified by column chromatography on silica gel (10 g)
- washeluted with dichloromethane
- customCombination and evaporation of suitable fractions