反应详情

612 mg of ethyl 2-[6-[3-[4-(diphenylmethylamino)piperidino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate was dissolved in 5 ml of ethanol; 2.2 ml of a 1 N aqueous solution of sodium hydroxide was added, followed by thermal refluxing for 6 hours. After cooling, the mixture was concentrated under reduced pressure. The residue was diluted with water, washed with ethyl acetate and adjusted to pH 5 by the addition of 1 N hydrochloric acid. The mixture was saturated with sodium chloride and extracted with tetrahydrofuran; the extract was dried over magnesium sulfate and concentrated under reduced pressure, powdered by the addition of ethyl ether, collected by filtration and dried to yield 503 mg of the title compound.

1. customrefluxing for 6 hours
2. temperatureAfter cooling
3. concentrationthe mixture was concentrated under reduced pressure
4. additionThe residue was diluted with water
5. washwashed with ethyl acetate
6. additionadjusted to pH 5 by the addition of 1 N hydrochloric acid
7. extractionextracted with tetrahydrofuran
8. dry with materialthe extract was dried over magnesium sulfate
9. concentrationconcentrated under reduced pressure
10. additionpowdered by the addition of ethyl ether
11. filtrationcollected by filtration
12. customdried