反应详情

温度

80 °C

A suspension of 0.80 (1.22 mmol) of tert-butyl 4-[3-[2-(benzhydrylideneamino)pyrid-4-yl]-2-(4-fluorophenyl)imidazo[1,2-b]pyridazin-6-yl]piperazine-1-carboxylate in 70 mL of aqueous hydrochloric acid is maintained at 80° C. for about 1 hour 30 minutes. After cooling, the aqueous phase is washed twice with diethyl ether and then basified by addition of ice-cold aqueous ammonia. The product is extracted with chloroform and the organic phase obtained is washed with water, dried over sodium sulfate and filtered, and the filtrate is concentrated under reduced pressure. The brown solid obtained is purified by chromatography on silica gel (35 g), eluting with a mixture of dichloromethane, methanol and aqueous ammonia (90/10/1). The product obtained is crystallized from 20 mL of refluxing acetonitrile to give 0.38 g of a white powder after cooling, filtering off and drying

1. temperatureAfter cooling
2. washthe aqueous phase is washed twice with diethyl ether
3. additionbasified by addition of ice-cold aqueous ammonia
4. extractionThe product is extracted with chloroform
5. customthe organic phase obtained
6. washis washed with water
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. concentrationthe filtrate is concentrated under reduced pressure
10. customThe brown solid obtained
11. customis purified by chromatography on silica gel (35 g)
12. washeluting with a mixture of dichloromethane, methanol and aqueous ammonia (90/10/1)
13. customThe product obtained
14. customis crystallized from 20 mL of refluxing acetonitrile