反应详情

温度

60 °C

1H-Indazole-3-carboxylic acid (5.0 g, 30.8 mmol) and carbonyl diimidazole (5.0 g, 33.9 mmol) were dissolved in N,N-dimethylformamide (150 mL) and heated to 60° C. After 2 hours, dimethylamine hydrochloride (4.0 g, 33.9) was added, and the reaction was stirred for an additional hour at 60° C. The reaction was poured into water, and the aqueous phase was extracted with ethyl acetate (3×150 mL). The combined organic phases were washed sequentially with aqueous sodium bicarbonate, 10% hydrochloric acid, water and brine. After drying over magnesium sulfate, filtering and concentrating in vacuo, the title compound was obtained.

1. extractionthe aqueous phase was extracted with ethyl acetate (3×150 mL)
2. washThe combined organic phases were washed sequentially with aqueous sodium bicarbonate, 10% hydrochloric acid, water and brine
3. dry with materialAfter drying over magnesium sulfate
4. filtrationfiltering
5. concentrationconcentrating in vacuo