反应详情

653 mg of ethyl 2-[3-chloro-6-[3-[4-(diphenylmethoxy)piperidino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate dihydrochloride was dissolved in 6 ml of ethanol; 1.97 ml of a 2 N aqueous solution of sodium hydroxide was added, followed by thermal refluxing for 2.5 hours. After cooling, 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 4.5 by the addition of 1 N hydrochloric acid. Acetone was added; the crystal precipitated was collected by filtration, washed with water-acetone (5:1) and dried to yield 465 mg of the title compound.

1. customrefluxing for 2.5 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. additionthe water layer was adjusted to pH 4.5 by the addition of 1 N hydrochloric acid
7. additionAcetone was added
8. customthe crystal precipitated
9. filtrationwas collected by filtration
10. washwashed with water-acetone (5:1)
11. customdried