Nitric Acid → 5-Nitro-1,10-phenanthroline

HRID 1180682

Reaktionsgleichung

Reaktionsgleichung von HRID 1180682
S(=O)(=O)(O)O.[N:6]1[C:19]2[C:10](=[CH:11][CH:12]=[C:13]3[C:18]=2[N:17]=[CH:16][CH:15]=[CH:14]3)[CH:9]=[CH:8][CH:7]=1.[N+:20]([O-])([OH:22])=[O:21].[OH-].[Na+]>O>[N+:20]([C:11]1[CH:12]=[C:13]2[C:18]([N:17]=[CH:16][CH:15]=[CH:14]2)=[C:19]2[C:10]=1[CH:9]=[CH:8][CH:7]=[N:6]2)([O-:22])=[O:21]

Komponenten

6

Edukt 4

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 13181,10-PhenanthrolineHCID 14798Sodium Hydroxide

Produkt 1

HCID 727905-Nitro-1,10-phenanthrolineAusbeute 68 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

Referring to Scheme 5, 237 ml sulfuric acid (concentrate) was first added to a 1 L three-necked flask. 35 g 1,10-phenanthroline was then added into the flask, and the temperature of mixture was kept lower than 100° C. Next, 2436 ml (67%) HNO3 was added drop by drop, and the temperature of mixture was kept lower than 110° C. The mixture was subsequently heated to 100° C. and stirred overnight. After completion of reaction, the reaction mixture was cooled to room temperature and placed into 2 L water, and then NaOH(aq) was added to adjust pH value to a range from 6 to 7, so as to give solids. The solids were washed by water, and dried to obtain solids 5-nitro-1,10-phenanthroline 30 g (0.13 mol, yield 68%).

Aufarbeitung

  1. additionwas first added to a 1 L three-necked flask
  2. customwas kept lower than 100° C
  3. customwas kept lower than 110° C
  4. customAfter completion of reaction
  5. temperaturethe reaction mixture was cooled to room temperature
  6. customso as to give solids
  7. washThe solids were washed by water
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-7ec48b0793ae48f98104c4ecd89ad208
Quelldatensatz
uspto-grants-2007_10
Patentnummer
US07282586B1

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