Sodium Hydroxide → 2-(2-Dimethylaminoethylamino)-5,6-dimethyl pyrazine

HRID 614310Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 614310
Cl[C:2]1[CH:7]=[N:6][C:5]([CH3:8])=[C:4]([CH3:9])[N:3]=1.[CH3:10][N:11]([CH2:13][CH2:14][NH2:15])[CH3:12].[OH-].[Na+]>O>[CH3:10][N:11]([CH3:12])[CH2:13][CH2:14][NH:15][C:2]1[CH:7]=[N:6][C:5]([CH3:8])=[C:4]([CH3:9])[N:3]=1

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 66053N,N-DimethylethylenediamineHCID 126003905-Chloro-2,3-dimethylpyrazine

Produkt 1

HCID 233499152-(2-Dimethylaminoethylamino)-5,6-dimethyl pyrazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

2-chloro-5,6-dimethylpyrazine (12.8 g., 0.09 mole) is added to unsym-dimethylethylenediamine (26 g., 0.295 mole) containing cuprous chloride (0.25 g.) and the mixture is heated for 48 hours in an oil bath maintained at 135°-140° C. On cooling, 50 ml of water and a single molar excess of 10N sodium hydroxide are added. The mixture is extracted with methylene chloride. The organic extracts are backwashed with saturated sodium chloride solution, dried over sodium sulfate, filtered and concentrated under vacuum. The residual oil is dissolved in hexane, filtered and reconcentrated to obtain the product oil (15.8 g., 0.081 mole).

Aufarbeitung

  1. temperaturethe mixture is heated for 48 hours in an oil bath
  2. temperaturemaintained at 135°-140° C
  3. temperatureOn cooling
  4. extractionThe mixture is extracted with methylene chloride
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum
  8. dissolutionThe residual oil is dissolved in hexane
  9. filtrationfiltered
  10. customto obtain the product oil (15.8 g., 0.081 mole)

Quellen und Nachweise

ORD-Eintrag
ord-717317f935e04e23a2f7aa78fd13bba6
Quelldatensatz
uspto-grants-1979_03
Patentnummer
US04144338

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