反应详情

温度

60 °C

To a solution of imidazo[1,2-b]pyridazine-6-amine (1.00 g, 7.45 mmol) and 4-dimethylaminopyridine (2.73 g, 22.4 mmol) in tetrahydrofuran (75 ml) was added 2,2,2-trichloroethyl chloroformate (3.09 ml, 22.4 mmol) with ice-cooling, and the mixture was stirred at 60° C. for 15 hours. Water was poured into the reaction solution, and the mixture was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. Hexane was added to the residue, and a solid was collected by filtration to give 1.92 g (53.1%) of the desired product.

1. temperaturecooling
2. extractionthe mixture was extracted with ethyl acetate
3. washThe extract was washed with water
4. dry with materialdried over anhydrous magnesium sulfate
5. distillationthe solvent was distilled off under reduced pressure
6. additionHexane was added to the residue
7. filtrationa solid was collected by filtration