Ethanol → HCID 178418578、化合物

HRID 5201ノート

反応式

HRID 5201 の反応式
[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]

参加物

5

反応物 3

HCID 702EthanolHCID 27242463-oxobutanoic acid lithium saltHCID 178418668HCID 178418668、化合物

生成物 1

HCID 178418578HCID 178418578、化合物収率 54.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-765eee938f5f4e1793095537f302f9ea
出典データセット
uspto-grants-1993_09
特許番号
US05243071

反応ノート

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