Ethyl Acetate → HCID 66679602, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of ethyl 3-iodo-1H-pyrazole-4-carboxylate (8.5 g, 32.0 mmol) in DMF (160 mL) was added 2,5-difluoropyridine (11.0 g, 96.0 mmol) and potassium carbonate (13.3 g, 96.0 mmol). The mixture was stirred at 100° C. in a sealed reaction flask. After 18 h, the mixture was cooled to ambient temperature and ethyl acetate and water were added. The solid in the organic layer was filtered off and the filtrate was dried over MgSO4, filtered and concentrated. The product was recrystallized using ethyl acetate and ether to give 6.5 g of the title compound. The solution from recrystallization was concentrated and purified by silica gel chromatography (100% dichloromethane→98% dichloromethane/methanol) gave 0.8 g of the title compound (7.3 g total). MS 361.8 (M+1).

Provenance & Evidence