反应详情

To a suspension of 2.30 g 6-chloro-3-(2,2,2-trifluoro-ethoxy)-pyridazin-4-ylamine in 23 ml dibromomethane was added 5.11 g isoamylnitrite at once and drop wise 4.642 g trimethylbromosilane at ambient temperature (during ca. 10 min). A moderate exotherm reaction was observed and a dark brown solution was obtained. The mixture was stirred at ambient temperature for 18 h. The solvents were evaporated and the residue was purified (3 times) by chromatography on silica gel using a gradient of heptane to dichloromethane to yield 0.70 g the title compound as white crystalline solid. MS (EI): 292 (M+H).

1. customat ambient temperature
2. custom(during ca. 10 min)
3. customA moderate exotherm reaction
4. customa dark brown solution was obtained
5. customThe solvents were evaporated
6. customthe residue was purified (3 times) by chromatography on silica gel using a gradient of heptane to dichloromethane