Nitric Acid → 2,3-Dinitrotoluene

HRID 259090

Reaktionsgleichung

Reaktionsgleichung von HRID 259090
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH3:10])([O-:3])=[O:2].[N+:11]([O-])([OH:13])=[O:12].S(=O)(=O)(O)O>C(Cl)Cl>[N+:11]([C:9]1[C:4]([N+:1]([O-:3])=[O:2])=[C:5]([CH3:10])[CH:6]=[CH:7][CH:8]=1)([O-:13])=[O:12]

Komponenten

5

Edukt 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 69442-Nitrotoluene

Produkt 1

HCID 117612,3-DinitrotolueneAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

68.6 g (0.5 mol) of 2-nitrotoluene were dissolved in 80 ml of methylene chloride and 38.6 g (0.6 mol) of 98% by weight nitric acid, followed by the addition under reflux with stirring over a period of 1 hour at boiling temperature of 40 g of 100% by weight sulphuric acid. After stirring for 2 hours under reflux, the methylene chloride phase was separated off without cooling and washed three times while still hot with 3 × 200 ml of water. After the washing water had been carefully separated off, the methylene chloride was distilled off, leaving 89.9 g (98% of the theoretical yield) of dinitrotoluene containing 99% of 2,4- and 2,6-dinitrotoluene.

Aufarbeitung

  1. temperatureunder reflux
  2. temperatureunder reflux
  3. customthe methylene chloride phase was separated off
  4. temperaturewithout cooling
  5. washwashed three times while still hot with 3 × 200 ml of water
  6. customAfter the washing water had been carefully separated off
  7. distillationthe methylene chloride was distilled off
  8. customleaving 89.9 g (98% of the

Quellen und Nachweise

ORD-Eintrag
ord-1ff2ed2186f145959a277f01e6c1d577
Quelldatensatz
uspto-grants-1977_07
Patentnummer
US04036838

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