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

HRID 1389689

Reaktionsgleichung

Reaktionsgleichung von HRID 1389689
[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

Edukt 3

HCID 1118Sulfuric AcidHCID 112881,2,3-Benzenetricarboxylic acidHCID 24434Potassium Nitrate

Produkt 1

HCID 144348595-Nitrobenzene-1,2,3-tricarboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

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 separated 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. customSome solid is separated out
  5. dissolutionis dissolved in water
  6. extractionThe entire aqueous mixture is extracted with ether
  7. washthe extract is washed with water
  8. dry with materialdried over magnesium sulfate
  9. concentrationThe ether is concentrated to a small volume, and petroleum ether
  10. additionis added
  11. customto precipitate a white solid
  12. customThe solid is collected
  13. customdried
  14. customto give 76.5 g

Quellen und Nachweise

ORD-Eintrag
ord-9a4621b2ee7641938a8fb46191b05c7f
Quelldatensatz
uspto-grants-1981_01
Patentnummer
US04245120

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