反应详情

To a solution, cooled to 0° C., of 5.20 g (21.0 mmol) of 6-chloro-2-(4-fluorophenyl)imidazo[1,2-b]pyridazine (CAS No.: 244081-70-7) in 130 mL of chloroform is rapidly added dropwise a solution of 6.61 g (40.9 mmol) of iodine monochloride in 40 mL of chloroform. After cooling to room temperature and stirring for 4 hours, the mixture is treated with aqueous 5% sodium thiosulfate solution. The product is extracted with dichloromethane. The organic phase is dried by filtration through a hydrophobic filter cartridge and concentrated under reduced pressure. The residue is triturated in acetonitrile, and the solid is isolated after filtering off and rinsing with diisopropyl ether. 5.7 g of a beige-colored powder are isolated after drying under vacuum.

1. extractionThe product is extracted with dichloromethane
2. customThe organic phase is dried by filtration through a hydrophobic filter cartridge
3. concentrationconcentrated under reduced pressure
4. customThe residue is triturated in acetonitrile
5. customthe solid is isolated
6. filtrationafter filtering off
7. washrinsing with diisopropyl ether