Hydrochloric Acid → HCID 20217061, compound

A solution of 1.0 g of imidazo-[1,2-a]-quinoline-2-carboxaldehye oxime in 100 ml of 0.25N methanolic hydrogen chloride in the presence of 0.100 g of 10% palladized carbon was hydrogenated at atmosphere pressure for 4 hours and after 175 ml of hydrogen were absorbed, 0.200 g of additional catalyst were added thereto. The mixture was hydrogenated further at 50° C. under atmosphere pressure for 2 hours during which 62 ml of hydrogen were absorbed. The mixture was filtered through cellulose powder and the filtrate was concentrated under reduced pressure. Anhydrous ether was added to the concentrate which was then cooled in ice to induce crystallization. The mixture was filtered and the recovered product was dried at 50° C. under vacuo and was crystallization from a methanol-ether mixture to obtain 0.85 g of imidazo-[1,2-a]-quinoline-2-methanamine dihydrochloride in the form of hygroscopic colorless crystals melting at 320°-325° C. with decomposition.

1. customafter 175 ml of hydrogen were absorbed
2. addition0.200 g of additional catalyst were added
3. waitThe mixture was hydrogenated further at 50° C. under atmosphere pressure for 2 hours during which 62 ml of hydrogen
4. customwere absorbed
5. filtrationThe mixture was filtered through cellulose powder
6. concentrationthe filtrate was concentrated under reduced pressure
7. additionAnhydrous ether was added to the
8. concentrationconcentrate which
9. temperaturewas then cooled in ice
10. customcrystallization
11. filtrationThe mixture was filtered
12. customthe recovered product was dried at 50° C. under vacuo
13. customcrystallization from a methanol-ether mixture

ORD record

ord-754a06db9d99463c9fcb0ffc256348a5

Source dataset

uspto-grants-1984_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04474784