反应详情

To a stirred solution of 5-amino -1-(2,6-dichloro-4-trifluoromethylphenyl)-4-iodo-3-methylpyrazole (2.85 g) in tetrahydrofuran (35 ml) at 0° C. was added dropwise t-butylnitrite (2.33 ml). The reaction mixture was allowed to warm to room temperature and then heated under reflux for 1.5 hours. The reaction mixture was evaporated and the residue purified by column chromatography on silica gel eluted with dichloromethane: hexane (1:1). Combination and evaporation of suitable fractions provided a yellow oil which was further purified by column chromatography on silica gel eluted with dichloromethane: hexane (1:2). Combination and evaporation of suitable fractions provided the title compound as a white solid, m.p. 118.5-119.4° C.

1. temperatureheated
2. temperatureunder reflux for 1.5 hours
3. customThe reaction mixture was evaporated
4. customthe residue purified by column chromatography on silica gel
5. washeluted with dichloromethane: hexane (1:1)
6. customCombination and evaporation of suitable fractions
7. customprovided a yellow oil which
8. customwas further purified by column chromatography on silica gel
9. washeluted with dichloromethane: hexane (1:2)
10. customCombination and evaporation of suitable fractions