HRID1108838
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
CONDITIONS
反应条件
- 温度
- 65 °C
PROCEDURE
实验过程
To a solution of 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-(furan-3-yl)pyrazole (0.204 g) in tetrahydrofuran (3 ml) was added t-butyl nitrite (187.8 μl). The mixture was heated to 65° C. for 1 hour, then cooled and evaporated The residue was purified by column chromatography on silica gel (5 g) eluted with hexane containing increasing amounts of dichloromethane (up to 100%). Combination and evaporation of appropriate fraction gave the title compound as a white solid, m.p. 139° C.
WORKUP
后处理
- temperaturecooled
- customevaporated The residue
- customwas purified by column chromatography on silica gel (5 g)
- washeluted with hexane containing
- temperatureincreasing amounts of dichloromethane (up to 100%)
- customCombination and evaporation of appropriate fraction