Potassium Carbonate → 1263089-45-7

Participants

Reaction Conditions

Reaction Steps

To a dry 2 L three neck flask equipped with a thermo pocket and condenser was charged N-(3-methyl-2-pyridinyl)formamide (100 g), potassium carbonate (109.6 g), tetrabutylammonium bromide (4.73 g), isopropyl alcohol (7500 mL) and 2-chloro-5-(chloromethyl)thiazole (distilled, 123.9 g) under a nitrogen atmosphere. The reaction mixture was then heated to 73-75° C. and maintained at that temperature for 5.5 hours. The mixture was then cooled to 50° C., and 10% aqueous NaOH (880 g) was added via an addition funnel over a period of 20 minutes. The resulting turbid reaction mass was stirred at 57-60° C. for approximately 3.5 hours. Water (approximately 800 mL) was added over a period of 5 minutes to the reaction mixture; the reaction mixture was then cooled to 10° C. and stirred at 10° C. for 10 minutes. The slurry was filtered, and the resulting solids were washed with chilled water (2×200 mL), air-dried, and further dried under reduced pressure at 40° C. for 16 h to provide a white solid (134 g).

Provenance & Evidence