反应详情

温度

80 °C

To barium hydroxide octahydrate (14.5 g, 46.1 mmol) was added water (240 mL), and the mixture was stirred at 80° C. for 15 min. A solution of ethyl (6-iodoimidazo[1,2-b]pyridazin-2-yl)carbamate (10.2 g, 30.7 mmol) in N-methylpyrrolidone (80 mL) was added to the mixture, and the mixture was stirred at 120° C. for 8 hr. After cooling the mixture to room temperature, water (480 mL) was added to the mixture, and the mixture was stirred for 1 hr. The mixture was extracted twice with ethyl acetate/tetrahydrofuran, washed with saturated brine, dried over anhydrous magnesium sulfate, and filtrated. The solvent was evaporated under reduced pressure, diisopropyl ether was added to the residue, and the precipitated crystals were collected by filtration to give the title compound (6.1 g, 76%) as a brown powder.

1. stirringthe mixture was stirred at 120° C. for 8 hr
2. temperatureAfter cooling the mixture to room temperature
3. stirringthe mixture was stirred for 1 hr
4. extractionThe mixture was extracted twice with ethyl acetate/tetrahydrofuran
5. washwashed with saturated brine
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationfiltrated
8. customThe solvent was evaporated under reduced pressure, diisopropyl ether
9. additionwas added to the residue
10. filtrationthe precipitated crystals were collected by filtration