反应详情

In ethanol (10 ml) was dissolved (+)-7-(2,5-dichlorothiophen-3-yl)-4-methyl-5,6,7,8-tetrahydroquinolin-5-one (0.36 g), and to the mixture were added aminoguanidine hydrochloride (0.15 g), concentrated hydrochloric acid (0.29 ml) and water (0.29 ml). The mixture was refluxed for 4 hours, and under reduced pressure, the solvent was evaporated. The residue was dissolved in water, and the mixture was washed with ethyl acetate and concentrated under reduced pressure. The residue was heated in a little amount of ethanol, and the solution was cooled. Precipitated crystals were filtered off, and the mother liquor was concentrated to give crystals, which were recrystallized from water to give (+)-7-(2,5-dichlorothiophen-3-yl)-5-guanidinoimino-4-methyl-5,6,7,8-tetrahydroquinoline hydrochloride (Compound 110) (0.46 g) as colorless crystals.

1. temperatureThe mixture was refluxed for 4 hours
2. customunder reduced pressure, the solvent was evaporated
3. dissolutionThe residue was dissolved in water
4. washthe mixture was washed with ethyl acetate
5. concentrationconcentrated under reduced pressure
6. temperatureThe residue was heated in a little amount of ethanol
7. temperaturethe solution was cooled
8. customPrecipitated crystals
9. filtrationwere filtered off
10. concentrationthe mother liquor was concentrated
11. customto give crystals, which
12. customwere recrystallized from water