反应详情

(2-Fluoro-5-nitrophenylethynyl)trimethylsilane (8.8 g, 37.1 mmol) and 1,4-dioxane were added to a solution of 1,2,4,5-tetrazine (35 ml, 18.6 mmol, 0.53 M in dichloromethane). The dichloromethane was distilled off and the dioxane solution was stirred at reflux for 36 hours. The solvent was removed to leave a brown oil. Purification by chromatography on silica gel eluting with dichloromethane, then with dichloromethane containing 1% methanol, gave 4-(2-fluoro-5-nitrophenyl)-5-trimethylsilanylpyridazine as a brown oil: m/z (ES+) 292 (M++H) and 249 (M+-3CH2).

1. distillationThe dichloromethane was distilled off
2. temperatureat reflux for 36 hours
3. customThe solvent was removed
4. customto leave a brown oil
5. customPurification by chromatography on silica gel eluting with dichloromethane