反应详情

温度

35 °C

Under a stream of argon, 1,10-phenanthroline (23 g; 127 mmol) was dissolved in nitrobenzene (500 mL). To the reaction mixture, methyl iodide (45.29 g; 319 mmol) was added dropwise at 35° C. over 3.5 hours. The resulting reaction mixture was stirred at 35° C. for 24 hours. The reaction mixture was cooled in an ice bath, filtered out. The resulting solids were sequentially washed with nitrobenzene, benzene, and ethanol, and evaporated under reduced pressure to give 36 g (yield: 88%) of the title compound (1).

1. customThe resulting reaction mixture
2. temperatureThe reaction mixture was cooled in an ice bath
3. filtrationfiltered out
4. washThe resulting solids were sequentially washed with nitrobenzene, benzene, and ethanol
5. customevaporated under reduced pressure