反应详情

A solution of 6.61 g (40.9 mmol) of iodine monochloride in 40 ml of chloroform is added in a rapid dropwise manner 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 number: 244081-70-7) in 130 ml of chloroform. After returning to ambient temperature and after stirring for 4 hours, the mixture is treated with a 5% aqueous solution of sodium thiosulphate. The product is extracted with dichloromethane, the organic phase is dried by filtration over a hydrophobic filtration cartridge and concentrated under reduced pressure. The residue is triturated in acetonitrile, the solid is isolated after filtration and rinsing with diisopropyl ether. 5.7 g of beige powder are isolated after drying under vacuum.

1. customAfter returning to ambient temperature
2. extractionThe product is extracted with dichloromethane
3. customthe organic phase is dried by filtration over a hydrophobic filtration cartridge
4. concentrationconcentrated under reduced pressure
5. customThe residue is triturated in acetonitrile
6. customthe solid is isolated
7. filtrationafter filtration
8. washrinsing with diisopropyl ether