反应详情

2.5 g (12.9 mmol) of 1-methyl-3-trifluoromethyl-1H-pyrazole-4-carboxylic acid in 25 mL of N,N-dimethylformanid (DMF) and 2.1 g (12.9 mmol) of N,N′-carbonyl diimidazole (CDI) were stirred at ambient temperature for 1 hour prior to addition of 1.2 g (12.9 mmol) of 3-aminopyridine. After three days of stirring the solvent was evaporated, the residue dissolved in dichloromethane, washed twice with a saturated solution of NaHCO3 and water. The combined organic phases were evaporated and the crude product was purified by flash column chromatography (silica using dichloromethane/methanol=95/5) to give 1.33 g (48%) of the title compound.

1. customwas evaporated
2. dissolutionthe residue dissolved in dichloromethane
3. washwashed twice with a saturated solution of NaHCO3 and water
4. customThe combined organic phases were evaporated
5. customthe crude product was purified by flash column chromatography (silica using dichloromethane/methanol=95/5)