Dimethylformamide → HCID 68486955, compound

Participants

Reaction Conditions

Reaction Steps

4-Nitropyridine-N-oxide (84.00 g), 4-Trifluoromethoxyphenol (107.8 g), K2CO3 (165.7 g) and DMF (420 mL) were placed in a vessel and stirred at 80-90° C. for 4.5 hr. The reaction mixture was then cooled to room temperature and water (2500 mL) and ethyl acetate (2500 mL) were added. The organic material was taken up in ethyl acetate and then the aqueous layer was extracted with ethyl acetate (1000 mL). The all organic extracts were washed three times with water (1000 mL×3). And then the organic extracts were condensed under reduced pressure to give the crude products (150.7 g). The crude products (150.7 g) and n-hexane (1500 mL) were placed in a vessel and stirred at 60° C. for 0.5 hr and then the mixture was allowed to cool to under 10° C. for 1 hr. The mixture was then filtered and the crystalline powder washed with n-hexane (168 mL) and dried at 50° C. for 17 hr to afford 139.4 g (85.73% yield) of a brown crystal target compound.

Provenance & Evidence