HRID5201
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
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.
WORKUP
后处理
- temperatureThe solution was heated
- temperatureto reflux over 30 minutes
- temperatureto cool
- wait, then at 4° C. for 24 hrs
- customto reach room temperature
- filtrationfiltered
- concentrationThe filtrate was concentrated to a paste
- customtriturated with 5 ml ethanol
- filtrationFiltration
- washwashing with ethanol