반응 #5297

반응 방정식

Lithium acetoacetate

aminoguanidine HCl

Ethanol

→

hydrazone

수율 54.9%

Acetoacetic Acid Guanylhydrazone

수율 54.9%

용매

water

water

반응 조건

후처리

1. 1
   온도The solution was heated
2. 2
   온도to reflux over 30 minutes
3. 3
   온도to cool
4. 4
   workup.WAIT, then at 4° C. for 24 hrs
5. 5
   기타to reach room temperature
6. 6
   여과filtered
7. 7
   농축The filtrate was concentrated to a paste
8. 8
   기타triturated with 5 ml ethanol
9. 9
   여과Filtration
10. 10
    세척washing with ethanol

실험 절차

Lithium acetoacetate (0.655 g) in 2 ml water 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 g of the hydrazone as a microcrystalline powder, melting point 138.6°-140° C.

출처