反应详情

温度

75 °C

tert-Butyl 3-methyl-1H-pyrazolo[3,4-b]pyridin-1-carboxylate (6.6 g, 28.3 mmol) was added into trifluoromethylbenzene (300 mL), and heated to 75° C. Then NBS (5.04 g, 28.3 mmol) was added, and after 15 minutes AIBN (465 mg, 2.8 mmol) was added, and heated to 80° C. and reacted for 1 hour. It was cooled slowly to room temperature and reacted for 12 hours. It was filtered to remove solid. The filtrate was rotate evaporated to dryness, and chromatographed on a column (PE:EA=25:1) to obtain a white solid 730 mg, at a yield of 8.3%.

1. temperatureheated to 80° C.
2. customreacted for 1 hour
3. temperatureIt was cooled slowly to room temperature
4. customreacted for 12 hours
5. filtrationIt was filtered
6. customto remove solid
7. customThe filtrate was rotate evaporated to dryness
8. customchromatographed on a column (PE:EA=25:1)