N,N-Dimethylaniline → 2-Butyrylamino-4-methyl-3-nitropyridine

HRID 248368

Reaktionsgleichung

Reaktionsgleichung von HRID 248368
[NH2:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([CH3:11])[CH:5]=[CH:4][N:3]=1.CN(C)C1C=CC=CC=1.[C:21](Cl)(=[O:25])[CH2:22][CH2:23][CH3:24]>C(OCC)(=O)C>[C:21]([NH:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([CH3:11])[CH:5]=[CH:4][N:3]=1)(=[O:25])[CH2:22][CH2:23][CH3:24]

Komponenten

5

Edukt 3

HCID 949N,N-DimethylanilineHCID 8855Butyryl chlorideHCID 2431662-Amino-4-methyl-3-nitropyridine

Produkt 1

HCID 214642392-Butyrylamino-4-methyl-3-nitropyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of 2-amino-4-methyl-3nitropyridine (5.0 g) and N,N-dimethylaniline (8.5 ml) was heated at 100° C. under nitrogen atmosphere. To the solution was added butyryl chloride (3.5 ml) and the mixture was stirred at 100° C. for 5 hours. After being cooled to room temperature, ethyl acetate was added to the reaction mixture. The organic layer was separated and washed successively with water and brine. The solution was dried over magnesium sulfate and the solvent was evaporated in vacuo. The residue was washed with n-hexane to give 2-butyrylamino-4-methyl-3-nitropyridine (7.0 g).

Aufarbeitung

  1. temperatureAfter being cooled to room temperature
  2. customThe organic layer was separated
  3. washwashed successively with water and brine
  4. dry with materialThe solution was dried over magnesium sulfate
  5. customthe solvent was evaporated in vacuo
  6. washThe residue was washed with n-hexane

Quellen und Nachweise

ORD-Eintrag
ord-9777e84daa0943d1869c526e16dd47ee
Quelldatensatz
uspto-grants-1993_05
Patentnummer
US05210092

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