Reaktion #1115218

ord-5c04f665d5c342628a4a89a4292bdec3

Lösungsmittel

Reaktionsbedingungen

Temperatur
20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturmaintained
  2. 2
    TemperaturThe reaction mixture is refluxed for 6 hours
  3. 3
    Filtrationfiltered
  4. 4
    EinengenThe filtrate is concentrated under reduced pressure
  5. 5
    Filtrationfiltered again
  6. 6
    Einengenconcentrated under reduced pressure
  7. 7
    Sonstige9.6 g of methyldimethylpyrazine chloride are recovered in the form of a mixture, which
  8. 8
    Sonstigeis used without further purification in the following step

Vorschrift

7.6 g (32.74 mmol) of trichloroisocyanuric acid are added, over 1 hour, to a solution, maintained at reflux, of 10 g of trimethylpyrazine (81.85 mmol) in 820 ml of dichloroethane. The reaction mixture is refluxed for 6 hours and then cooled to 20° C., stirred for a further 12 hours and filtered. The filtrate is concentrated under reduced pressure, taken up in 200 ml of ethyl ether, filtered again and then concentrated under reduced pressure. 9.6 g of methyldimethylpyrazine chloride are recovered in the form of a mixture, which is used without further purification in the following step.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08735432B2uspto-grants-2014_05