Sulfuric Acid → 2,3,5-Trimethylpyridine

HRID 2231949Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2231949
Cl[C:2]1[C:7]([CH3:8])=[C:6](Cl)[N:5]=[C:4]([CH3:10])[C:3]=1[CH3:11].OS(O)(=O)=O>C(O)C.[Zn]>[CH3:10][C:4]1[C:3]([CH3:11])=[CH:2][C:7]([CH3:8])=[CH:6][N:5]=1

Komponenten

5

Edukt 2

HCID 1118Sulfuric AcidHCID 27791392,4-Dichloro-3,5,6-trimethylpyridine

Produkt 1

HCID 127592,3,5-Trimethylpyridine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23994ZincKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

3,8 g (20 mmoles) of 4.6-dichloro-2,3,5-trimethylpyridine are dissolved in a small amount of ethanol and treated with 5 g of zinc powder. After addition of 10 ml of 2 N H2SO4, the mixture is refluxed for 1 hour. After cooling and filtering the solution is treated with NaOH to adjust a pH of 6. The precipitated zinc salts are removed by filtration and the filtrate is extracted three times with petrol ether. After drying and evaporation 2.0 g (83%) of 2,3,5-trimethylpyridine are obtained.

Aufarbeitung

  1. temperaturethe mixture is refluxed for 1 hour
  2. temperatureAfter cooling
  3. filtrationfiltering the solution
  4. additionis treated with NaOH
  5. customThe precipitated zinc salts are removed by filtration
  6. extractionthe filtrate is extracted three times with petrol ether
  7. customAfter drying
  8. customevaporation 2.0 g (83%) of 2,3,5-trimethylpyridine
  9. customare obtained

Quellen und Nachweise

ORD-Eintrag
ord-34cdf6932df9494598878de3cecc58af
Quelldatensatz
uspto-grants-1988_11
Patentnummer
US04785113

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