Reaktion #365167

ord-ce861ade785846d4b549f7d2f2c21d94

Reaktionsgleichung

Cc1nc(N)ccc1[N+](=O)[O-]
2-amino-5-nitro-6-methylpyridine
O=S(=O)(O)O
sulfuric acid
O=[N+]([O-])[O-].[Na+]
sodium nitrate
Cc1[nH]c(=O)ccc1[N+](=O)[O-]
title compound
Ausbeute 97.0%
Cc1[nH]c(=O)ccc1[N+](=O)[O-]
2-Oxo-5-Nitro-6-Methyl-1,2-Dihydropyridine
Ausbeute 97.0%

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added
  2. 2
    TemperaturThe reaction mixture was warmed to room temperature over 4 hours
  3. 3
    Temperaturcooled to 0° C
  4. 4
    SonstigeThe resulting ivory precipitate was collected
  5. 5
    Waschenwashed with cold water
  6. 6
    Sonstigedried at 40° C. in vacuo overnight

Vorschrift

To a suspension of 2-amino-5-nitro-6-methylpyridine (40.24 g, 260 mmol) was added concentrated sulfuric acid (48 mL). The homogeneous solution was cooled to 0° C., and sodium nitrate (26.97 g, 390 mmol) dissolved in 120 mL of water was added. The reaction mixture was warmed to room temperature over 4 hours, then cooled to 0° C. The resulting ivory precipitate was collected, washed with cold water, and dried at 40° C. in vacuo overnight to provide 39.05 g (97%) of the title compound. EA calculated for C6H6N2O3: C, 46.76; H, 3.92; N, 18.18. Found: C, 46.49; H, 3.94; N, 17.99.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06358972B1uspto-grants-2002_03