Ethanol → HCID 178418578, 화합물

HRID 5201노트

반응식

HRID 5201 반응식
[C:1]([O-:7])(=[O:6])[CH2:2][C:3]([CH3:5])=O.[Li+].[C:9]([NH:12][NH2:13])([NH2:11])=[NH:10].Cl.C(O)C>O>[C:9]([NH:12][N:13]=[C:3]([CH3:5])[CH2:2][C:1]([OH:7])=[O:6])(=[NH:10])[NH2:11]

참가 물질

5

반응물 3

HCID 702EthanolHCID 27242463-oxobutanoic acid lithium saltHCID 178418668HCID 178418668, 화합물

생성물 1

HCID 178418578HCID 178418578, 화합물수율 54.9%

시약·촉매·용매 1

HCID 962Water용매2회

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.

후처리

  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

출처 및 근거

ORD 기록
ord-765eee938f5f4e1793095537f302f9ea
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05243071

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