Sulfuric acid magnesium salt (1:1) → N-[3-(3-Methoxyphenyl)propylidene]-N'-(4-pyridinyl)hydrazine hydrochloride

HRID 612453

Reaktionsgleichung

Reaktionsgleichung von HRID 612453
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][CH:11]=O)[CH:6]=[CH:7][CH:8]=1.[ClH:13].[NH:14]([C:16]1[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=1)[NH2:15].S([O-])([O-])(=O)=O.[Mg+2]>C(O)C>[ClH:13].[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][CH:11]=[N:15][NH:14][C:16]2[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=2)[CH:6]=[CH:7][CH:8]=1

Komponenten

5

Edukt 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 114237693-(3-Methoxyphenyl)propionaldehydeHCID 223202584-Hydrazinylpyridine hydrochloride

Produkt 1

HCID 70107610N-[3-(3-Methoxyphenyl)propylidene]-N'-(4-pyridinyl)hydrazine hydrochlorideAusbeute 61 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A slurry of 3-(3-methoxyphenyl)propionaldehyde (6.46 g), 4-hydrazinopyridine hydrochloride (6.30 g) and magnesium sulfate (5 g) in ethanol (75 ml) was heated under reflux, under nitrogen, with stirring, for 45 mins. The reaction mixture was filtered, the filter cake was washed with ethyl acetate, and the filtrate was concentrated in vacuo. The residue was triturated with ethyl acetate to give 7 g (61%) of product, mp 155-156° C.

Aufarbeitung

  1. temperatureunder reflux, under nitrogen
  2. filtrationThe reaction mixture was filtered
  3. washthe filter cake was washed with ethyl acetate
  4. concentrationthe filtrate was concentrated in vacuo
  5. customThe residue was triturated with ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-94ca095354cf45b59cf18d606a9ab0bc
Quelldatensatz
uspto-grants-1999_12
Patentnummer
US06004977

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