反应详情

In 8 mL of ethanol, 1.667 g of the ethyl 2-[6-[3-[4-(diphenylmethoxy)piperidino]propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate synthesized in Reference Example 2C was dissolved, and 0.631 g of citric acid monohydrate was added thereto and dissolved under heating, followed by concentration under reduced pressure. To the residue was added 23 mL of ethyl acetate, and the crystals formed were collected by filtration and washed with 12 mL of ethyl acetate. To the crystals was added 30 mL of methanol and the crystals were dissolved under heating, followed by concentration under reduced pressure. To the residue was added 30 mL of ethanol and the residue was then dissolved. After still standing, the crystals formed were collected by filtration, washed with 10 mL of ethanol and dried to yield 2.007 g of the title compound.

1. dissolutionwas dissolved
2. dissolutiondissolved
3. temperatureunder heating
4. concentrationfollowed by concentration under reduced pressure
5. additionTo the residue was added 23 mL of ethyl acetate
6. customthe crystals formed
7. filtrationwere collected by filtration
8. washwashed with 12 mL of ethyl acetate
9. additionTo the crystals was added 30 mL of methanol
10. dissolutionthe crystals were dissolved
11. temperatureunder heating
12. concentrationfollowed by concentration under reduced pressure
13. additionTo the residue was added 30 mL of ethanol
14. dissolutionthe residue was then dissolved
15. customthe crystals formed
16. filtrationwere collected by filtration
17. washwashed with 10 mL of ethanol
18. customdried