Nitric Acid → 2,9-Dimethyl-5-nitro-1,10-phenanthroline

HRID 257614

Reaktionsgleichung

Reaktionsgleichung von HRID 257614
[CH3:1][C:2]1[CH:15]=[CH:14][C:13]2[C:4](=[C:5]3[C:10](=[CH:11][CH:12]=2)[CH:9]=[CH:8][C:7]([CH3:16])=[N:6]3)[N:3]=1.[N+:17]([O-])([OH:19])=[O:18]>S(=O)(=O)(O)O>[N+:17]([C:11]1[CH:12]=[C:13]2[C:4]([N:3]=[C:2]([CH3:1])[CH:15]=[CH:14]2)=[C:5]2[C:10]=1[CH:9]=[CH:8][C:7]([CH3:16])=[N:6]2)([O-:19])=[O:18]

Komponenten

4

Edukt 2

HCID 944Nitric AcidHCID 652372,9-Dimethyl-1,10-phenanthroline

Produkt 1

HCID 3797642,9-Dimethyl-5-nitro-1,10-phenanthroline

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

2,9-Dimethyl-1,10-phenanthroline (h) (20 g) was dissolved in a mixture of sulfuric acid (120 ml) and nitric acid (40 ml), and the mixture was heated at 100° C. for 12 hours with stirring. The resulting solution was poured into ice water (300 ml), and the formed precipitate was collected. The precipitate was dissolved in water (500 ml) and neutralized with sodium hydroxide. The resulting precipitate was collected and recrystallized from methanol (300 ml) to give the desired 5-nitro-2,9-dimethyl-1,10-phenanthroline (i) (yield=8.8 g).

Aufarbeitung

  1. customthe formed precipitate was collected
  2. dissolutionThe precipitate was dissolved in water (500 ml)
  3. customThe resulting precipitate was collected
  4. customrecrystallized from methanol (300 ml)

Quellen und Nachweise

ORD-Eintrag
ord-5decf9e2f16549c0a64c2625484c21b4
Quelldatensatz
uspto-grants-1993_11
Patentnummer
US05262526

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