Reaktion #161261

ord-591ef915f90248d5a52584cd39a6e0b2

Reaktionsgleichung

N
ammonia
Cn1cc([N+](=O)[O-])cc([N+](=O)[O-])c1=O
1-methyl-3,5-dinitro-2-pyridone
CC(=O)C(C)C
3-methyl-2-butanone
CC(C)c1ccc([N+](=O)[O-])cn1
2-isopropyl-5-nitro-pyridine
Ausbeute 28.3%

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was removed under vacuum
  2. 2
    workup.DISSOLUTIONthe residual oil was dissolved in CH2Cl2
  3. 3
    Filtrationfiltered
  4. 4
    TrocknenThe filtrate was dried over Na2SO4
  5. 5
    Einengenconcentrated

Vorschrift

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%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08829204B2uspto-grants-2014_09