反应详情

温度

80 °C

To a solution of 5-(2,4-difluorophenoxy)-1-isobutyl-1H-indazol-6-ol (0.015 g, 0.05 mmol) in DMF (1 mL) was added Cs2CO3. The reaction mixture was stirred for 30 minutes before the addition of 1-bromo-3-chloropropane (0.01 g, 0.08 mmol) and then was heated to 80° C. for 25 hours. After cooling the mixture to room temperature, the reaction mixture was diluted with water and ether and the layers separated. The aqueous layer was extracted with ether and the combined organic layers were washed with 1N NaOH, water, and brine. The crude mixture was dried over Na2SO4 and concentrated under reduced pressure to afford the product with a small impurity. The crude mixture was used in the next reaction without further purification.

1. temperatureAfter cooling the mixture to room temperature
2. customthe layers separated
3. extractionThe aqueous layer was extracted with ether
4. washthe combined organic layers were washed with 1N NaOH, water, and brine
5. dry with materialThe crude mixture was dried over Na2SO4
6. concentrationconcentrated under reduced pressure
7. customto afford the product with a small impurity