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Potassium Nitrate → HCID 178430971, Verbindung

HRID 968793
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 968793
[CH3:1][C:2]1[C:7]2[NH:8][CH:9]=[N:10][C:6]=2[C:5]([C:11]([OH:13])=[O:12])=[CH:4][CH:3]=1.[N+:14]([O-])([O-:16])=[O:15].[K+]>OS(O)(=O)=O>[CH3:1][C:2]1[C:7]2[NH:8][CH:9]=[N:10][C:6]=2[C:5]([C:11]([OH:13])=[O:12])=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 24434Potassium NitrateHCID 178425875HCID 178425875, Verbindung

Produkt 1

HCID 178430971HCID 178430971, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

A mixture of 7-Methyl-1H-benzimidazole-4-carboxylic Acid (22) (4.944 g, 28.10 mmol) and concentrated H2SO4 (30 mL) is heated to about 60° C. to obtain a solution which is then cooled to about 0° C. To this solution is added KNO3 (3.12 g, 30.9 mmol) portionwise, so as to maintain the internal reaction temperature <10° C. Following complete addition, the cooling source is removed and the reaction mixture is allowed to warm to ambient temperature, whereupon the mixture is stirred for about 1 hour. The reaction mixture is then added to ice water (100 mL) and held at about 0° C. for about 4 hours. The resulting solids are filtered, washed with water, and dried to provide 7-Methyl-6-nitro-1H-benzimidazole-4-carboxylic Acid (23) as an off white solid (6.12 g, 98% yield).

Aufarbeitung

  1. customto obtain a solution which
  2. temperatureis then cooled to about 0° C
  3. temperatureso as to maintain the internal reaction temperature <10° C
  4. additionaddition
  5. customthe cooling source is removed
  6. temperatureto warm to ambient temperature, whereupon the mixture
  7. additionThe reaction mixture is then added to ice water (100 mL)
  8. waitheld at about 0° C. for about 4 hours
  9. filtrationThe resulting solids are filtered
  10. washwashed with water
  11. customdried

Quellen und Nachweise

ORD-Eintrag
ord-c4772c6d3e6b4a3b8a5c8ae286d5b590
Quelldatensatz
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07304084B2

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