反应详情

温度

150 °C

The mixture of 0.90 g (2.8 mmol) of 6-chloro-2-(4-fluorophenyl)-3-(pyridazin-4-yl)-imidazo[1,2-b]pyridazine and 1.7 g (8.3 mmol) of 5-benzyloctahydropyrrolo[3,4-c]pyrrole in 15 ml of pentanol is heated in a sealed tube at 150° C. for 18 hours. The reaction medium is poured into a 1N aqueous solution of hydrochloric acid and the aqueous phase is washed with ethyl acetate. The aqueous phase is then basified using aqueous sodium hydroxide and the product is extracted with dichloromethane. The organic phase is dried over sodium sulfate and then concentrated under reduced pressure. The product is chromatographed on a silica gel column, elution being carried out with a mixture of aqueous ammonia, methanol and dichloromethane (0.2/2/98), to give 1.2 g of solid in the form of an amorphous white foam.

1. washthe aqueous phase is washed with ethyl acetate
2. extractionthe product is extracted with dichloromethane
3. dry with materialThe organic phase is dried over sodium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe product is chromatographed on a silica gel column, elution
6. additionbeing carried out with a mixture of aqueous ammonia, methanol and dichloromethane (0.2/2/98)