Ammonia → 2-Isopropyl-5-nitropyridine

HRID 401411

Reaktionsgleichung

Reaktionsgleichung von HRID 401411
C[N:2]1[CH:7]=[C:6]([N+]([O-])=O)[CH:5]=[C:4]([N+:11]([O-:13])=[O:12])[C:3]1=O.[CH3:15][CH:16](C)[C:17](=O)C.N>CO>[CH:16]([C:7]1[CH:6]=[CH:5][C:4]([N+:11]([O-:13])=[O:12])=[CH:3][N:2]=1)([CH3:17])[CH3:15]

Komponenten

5

Edukt 3

HCID 222AmmoniaHCID 112513-Methyl-2-butanoneHCID 36212361-Methyl-3,5-dinitro-1H-pyridin-2-one

Produkt 1

HCID 450963212-Isopropyl-5-nitropyridineAusbeute 28,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel2×

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

To a solution of 1-methyl-3,5-dinitro-2-pyridone (8.0 g, 40 mmol) in methyl alcohol (20 mL) was added dropwise 3-methyl-2-butanone (5.1 mL, 48 mmol), followed by ammonia solution in methyl alcohol (10.0 g, 17%, 100 mmol). The reaction mixture was heated at 70° C. for 2.5 h under atmospheric pressure. The solvent was removed under vacuum and the residual oil was dissolved in CH2Cl2, and then filtered. The filtrate was dried over Na2SO4 and concentrated to afford 2-isopropyl-5-nitro-pyridine (1.88 g, 28%).

Aufarbeitung

  1. customThe solvent was removed under vacuum
  2. dissolutionthe residual oil was dissolved in CH2Cl2
  3. filtrationfiltered
  4. dry with materialThe filtrate was dried over Na2SO4
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-c54b587836da45ddaf467f7055924490
Quelldatensatz
uspto-grants-2014_06
Patentnummer
US08741925B2

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