Ethanol → HCID 178418414, Verbindung

HRID 2344

Reaktionsgleichung

Reaktionsgleichung von HRID 2344
[H-].[Na+].Cl.[C:4]([NH2:10])(=[NH:9])[CH2:5][CH2:6][CH2:7][CH3:8].[CH:11]([CH:13]=[CH:14][C:15]([O:17][CH3:18])=[O:16])=O.[CH2:19](O)C>C1C=CC=CC=1>[CH2:5]([C:4]1[NH:9][CH:11]=[C:13]([CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16])[N:10]=1)[CH2:6][CH2:7][CH3:8]

Komponenten

6

Edukt 4

HCID 702EthanolHCID 24758Sodium hydrideHCID 111293Methyl 4-oxobut-2-enoateHCID 11615174Pentanimidamide Hydrochloride

Produkt 1

HCID 178418414HCID 178418414, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

Sodium hydride (2.82 g, 0,117 mol) was dissolved in 30 ml of absolute ethanol at 0° C. Valeramidine hydrochloride (16.71 g, 0.123 mol) was added to this solution, and after 15 minutes the solution was filtered and the collected solid was washed with 20 ml of ethanol and 50 ml of benzene. The combined filtrates were diluted with 750 ml of benzene, 15 g (0.117 mol) of methyl 3-formylacrylate was added, and the mixture was refluxed for 18.5 h using a trap to remove water. The solvents were removed under vacuum and the residue slurried in ether. Evaporation of the ether solution gave the title compound as an oil.

Aufarbeitung

  1. filtrationafter 15 minutes the solution was filtered
  2. washthe collected solid was washed with 20 ml of ethanol and 50 ml of benzene
  3. additionwas added
  4. temperaturethe mixture was refluxed for 18.5 h
  5. customto remove water
  6. customThe solvents were removed under vacuum
  7. customEvaporation of the ether solution

Quellen und Nachweise

ORD-Eintrag
ord-2843bd13368f422ab3826093b175bc25
Quelldatensatz
uspto-grants-1998_03
Patentnummer
US05728842

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