反应详情

Lithium acetoacetate (0.655 g) in 2 ml water was treated with 0.665 g aminoguanidine HCl in 1.33 ml water. The solution was heated to reflux over 30 minutes and then allowed to cool. Ethanol (10 ml) was added and the mixture was stored at -20° C. for 24 hrs., then at 4° C. for 24 hrs. The mixture was allowed to reach room temperature and filtered. The filtrate was concentrated to a paste and triturated with 5 ml ethanol. Filtration and washing with ethanol gave 0.522 to the hydrazone as a microcrystalline powder, melting point 138.6°-140° C.

1. temperatureThe solution was heated
2. temperatureto reflux over 30 minutes
3. temperatureto cool
4. wait, then at 4° C. for 24 hrs
5. customto reach room temperature
6. filtrationfiltered
7. concentrationThe filtrate was concentrated to a paste
8. customtriturated with 5 ml ethanol
9. filtrationFiltration
10. washwashing with ethanol