反应详情

468 mg of ethyl 2-[6-[3-[4-(diphenylmethoxy)piperidino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate was dissolved in 3 ml of ethanol; 2 ml of a 1 N aqueous solution of sodium hydroxide was added, followed by stirring at room temperature for 15 hours. After the mixture was concentrated under reduced pressure. The residue was diluted with water and washed with ethyl acetate; the water layer was adjusted to pH 7 by the addition of 1 N hydrochloric acid, followed by extraction with ethyl acetate-tetrahydrofuran (1:1); the extract was washed with saturated saline, dried over magnesium sulfate and concentrated under reduced pressure. Ethyl acetate was added to the residue; the crystal precipitated was collected by filtration, washed with ethyl acetate and dried to yield 267 mg of the title compound.

1. concentrationAfter the mixture was concentrated under reduced pressure
2. additionThe residue was diluted with water
3. washwashed with ethyl acetate
4. additionthe water layer was adjusted to pH 7 by the addition of 1 N hydrochloric acid
5. extractionfollowed by extraction with ethyl acetate-tetrahydrofuran (1:1)
6. washthe extract was washed with saturated saline
7. dry with materialdried over magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. additionEthyl acetate was added to the residue
10. customthe crystal precipitated
11. filtrationwas collected by filtration
12. washwashed with ethyl acetate
13. customdried