反应详情

温度

90 °C

A solution of 1-methyl-5-pyridin-2-yl-1H-pyrazole-3-carboxylic acid (205 mg, 1.0 mmol) in tert-butanol (3.8 ml) was treated with diphenylphosphoryl azide (225 μl, 1.0 mmol) and triethylamine (280 μl, 2.0 mmol) and stirred at 90° C. for 24 hours. Since the reaction was not completed, another equivalent of diphenylphosphoryl azide (225 μl) and two equivalents of triethylamine (280 μl) were added and stirring was continued at 90° C. for another 24 hours. The crude product was purified by silica gel chromatography using a heptane/ethyl acetate gradient and the final product was obtained as off-white solid (66 mg, 24%).

1. stirringstirring
2. waitwas continued at 90° C. for another 24 hours
3. customThe crude product was purified by silica gel chromatography