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Methylhydrazine → HCID 19917929, Verbindung

HRID 1755872
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1755872
CNN.[OH:4][C:5]1[C:6](=[O:25])[N:7]([CH3:24])[C:8]([CH2:11][O:12][N:13]2C(=O)C3=CC=CC=C3C2=O)=[N:9][CH:10]=1>CN(C)C=O>[NH2:13][O:12][CH2:11][C:8]1[N:7]([CH3:24])[C:6](=[O:25])[C:5]([OH:4])=[CH:10][N:9]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 6061MethylhydrazineHCID 19918009HCID 19918009, Verbindung

Produkt 1

HCID 19917929HCID 19917929, VerbindungAusbeute 73 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

Methylhydrazine (92 mg) (2 mmol) are added at 0° C. to a suspension of 301 mg (1 mmol) of N-[(3,4-dihydro-5-hydroxy-3-methyl-4-oxo-2-pyrimidinyl)methoxy]phthalimide in 9 ml of absolute dimethylformamide. A solution gradually results and this is then stirred at room temperature for 3 hours. The solution is concentrated in a high vacuum at room temperature, the residue is washed with petroleum ether and finally 10 ml of water are added thereto. After good intermixing the mixture is filtered. The filtrate is concentrated, finally with toluene/ethanol. After crystallization from ethanol there are obtained 125 mg of 2-[(aminooxy)methyl]-5-hydroxy-3-methyl-4(3H)-pyrimidinone as white crystals of m.p. 106° C.

Aufarbeitung

  1. customA solution gradually results
  2. concentrationThe solution is concentrated in a high vacuum at room temperature
  3. washthe residue is washed with petroleum ether and finally 10 ml of water
  4. additionare added
  5. filtrationAfter good intermixing the mixture is filtered
  6. concentrationThe filtrate is concentrated, finally with toluene/ethanol
  7. customAfter crystallization from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-77713f4599d64438b87fa4278811e8bf
Quelldatensatz
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05438052

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