Reaktion #48020
ord-f1156178cb0a47d3a158b5cf8a0dd4dc
Reaktionsgleichung
trichloroisocyanuric acid
trimethylpyrazine
→
(Chloromethyl)dimethylpyrazine
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturmaintained
- 2TemperaturThe reaction mixture is refluxed for 6 hours
- 3Filtrationfiltered
- 4EinengenThe filtrate is concentrated under reduced pressure
- 5Filtrationfiltered again
- 6Einengenconcentrated under reduced pressure
- 7Sonstige9.6 g of methyldimethylpyrazine chloride are recovered in the form of a mixture, which
- 8Sonstigeis 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.