Reaktion #1147805

ord-f360d075db0a4f93a9119f546655f1b6

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    Temperaturwhile cooling the reaction flask
  2. 2
    workup.ADDITIONAfter completion of addition
  3. 3
    workup.WAITfollowed by another 1 h at room temperature
  4. 4
    SonstigeA light pink solid was isolated by filtration
  5. 5
    Waschenwashed with cold water (100 mL)
  6. 6
    SonstigeThe solid was dried in a vacuum oven overnight

Vorschrift

Part A: 4,6-Dihydroxy-2-methylpyrimidine (60 g) was added in portions to fuming nitric acid (120 mL) at 0° C. while cooling the reaction flask. After completion of addition, the reaction was stirred an additional 1 h at 0° C. followed by another 1 h at room temperature. The reaction mixture was then poured over ice (200 g) and the ice was allowed to melt. A light pink solid was isolated by filtration and washed with cold water (100 mL). The solid was dried in a vacuum oven overnight to yield 4,6-dihydroxy-2-methyl-5-nitropyrimidine (72.5 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06525056B2uspto-grants-2003_02