1-Ethyl-2-methylpyridinium Bromide synthesis

Yield:32353-50-7 97%

Reaction Conditions:

at 95 - 100; under 112.511 - 300.03 Torr; for 3 h;Inert atmosphere;Sealed tube;Concentration;Pressure;Temperature;Time;Solvent;

Steps:

3 Example 3Preparation of 2-MEPy using a slight excess of 2-picoline

Example 3Preparation of 2-MEPy using a slight excess of 2-picolineA pressure reactor was equipped with a mechanical stirrer, a magnetic relay and a thermocouple well. The reactor was purged with nitrogen and charged with 2-picoline (662 g) . Vacuum was applied (0.15 bara) , the reactor was sealed and heated to 95 °C following which the pressure increased to about 0.4 bara. Ethyl bromide (763 g) was then added during 120 minutes, at 95-100 °C. Heating at 100 °C was continued for additional one hour (at the end of cooking period, the pressure was 0.4 bara) . Vacuum and dry evaporation were applied for 1 hour, in order to remove the residual 2-picoline. Water was then added (300 mL) and second vacuum distillation was performed (50 mL were removed) . The weight of the aqueous concentrate was 1605 g and the concentration of 2-MEPy 85 weight % (argentometric titration); yield, 97 %.

References:

WO2013/42109,2013,A1 Location in patent:Page/Page column 10