反应详情

0.810 g of N-[6-[3-[4-(diphenylmethoxy)piperidino]propylamino]imidazo[1,2-b]pyridazine-2-carbonyl]glycine ethyl ester was dissolved in 4 ml of ethanol; 2 ml of a 1 N aqueous solution of sodium hydroxide was added, followed by stirring at room temperature for 3 hours. The mixture was concentrated under reduced pressure; ice water and 2.1 ml of 1 N hydrochloric acid were added to the residue, followed by extraction with ethyl acetate-tetrahydrofuran (1:2); the extract was washed with saturated saline and dried with magnesium sulfate. The dry product was concentrated under reduced pressure; the residue was powdered by the addition of ethyl acetate, collected by filtration and washed with ethyl acetate to yield 0.183 g of the title compound.

1. concentrationThe mixture was concentrated under reduced pressure
2. additionice water and 2.1 ml of 1 N hydrochloric acid were added to the residue
3. extractionfollowed by extraction with ethyl acetate-tetrahydrofuran (1:2)
4. washthe extract was washed with saturated saline
5. dry with materialdried with magnesium sulfate
6. concentrationThe dry product was concentrated under reduced pressure
7. additionthe residue was powdered by the addition of ethyl acetate
8. filtrationcollected by filtration
9. washwashed with ethyl acetate