Sulfuric Acid → 5-Nitrobenzene-1,2,3-tricarboxylic acid

HRID 1389699

Reaktionsgleichung

Reaktionsgleichung von HRID 1389699
[C:1]1([C:13]([OH:15])=[O:14])[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([OH:9])=[O:8])[C:2]=1[C:10]([OH:12])=[O:11].S(=O)(=O)(O)O.[N+:21]([O-])([O-:23])=[O:22].[K+]>O>[N+:21]([C:5]1[CH:6]=[C:1]([C:13]([OH:15])=[O:14])[C:2]([C:10]([OH:12])=[O:11])=[C:3]([C:7]([OH:9])=[O:8])[CH:4]=1)([O-:23])=[O:22]

Komponenten

5

Versuchsvorschrift

To a stirred mixture of 125 g. of 1,2,3-benzenetricarboxylic acid and 900 ml. of concentrated sulfuric acid at 60°-70° C. is added, gradually over a 2 hour period, 312 g. of potassium nitrate. The mixture is heated at 135°-140° C. for 16 hours, cooled and treated with ice and water. Some solid is seprated out and is dissolved in water. The entire aqueous mixture is extracted with ether, the extract is washed with water and dried over magnesium sulfate. The ether is concentrated to a small volume, and petroleum ether is added to precipitate a white solid. The solid is collected and dried to give 76.5 g. of the product of the Example.

Aufarbeitung

  1. additionTo a stirred mixture of 125 g
  2. temperatureThe mixture is heated at 135°-140° C. for 16 hours
  3. temperaturecooled
  4. extractionThe entire aqueous mixture is extracted with ether
  5. washthe extract is washed with water
  6. dry with materialdried over magnesium sulfate
  7. concentrationThe ether is concentrated to a small volume, and petroleum ether
  8. additionis added
  9. customto precipitate a white solid
  10. customThe solid is collected
  11. customdried
  12. customto give 76.5 g

Quellen und Nachweise

ORD-Eintrag
ord-f6e7e0af7c074fe39bc516d750ab9f2f
Quelldatensatz
uspto-grants-1981_01
Patentnummer
US04245119

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