反应详情

温度

0 °C

3-(4-Methoxybenzyl)-6-phenyl-[1,2,4]triazolo[4,3-a]pyridine (0.057 g, 0.18 mmol) was dissolved in dichloromethane (2.5 mL) then cooled to 0° C. A 1M solution of boron tribromide (0.72 ml, 0.72 mmol) in dichloromethane was added slowly. The reaction mixture was stirred at 0° C. for 2 hours. A precipitate was present in the reaction mixture. The reaction was quenched with ice chips and stirred overnight at room temperature. A solid remained in the mixture. The reaction mixture was diluted with dichloromethane/methanol to give a clear mixture then washed with saturated aqueous sodium bicarbonate and brine. The organic layer was dried over sodium sulfate and concentrated under vacuum. The sample was purified by preparative TLC eluting with 7% methanol in dichloromethane which afforded 4-((6-phenyl-[1,2,4]triazolo[4,3-a]pyridin-3-yl)methyl)phenol as an off-white solid

1. customThe reaction was quenched with ice chips
2. stirringstirred overnight at room temperature
3. additionThe reaction mixture was diluted with dichloromethane/methanol
4. customto give a clear mixture
5. washthen washed with saturated aqueous sodium bicarbonate and brine
6. dry with materialThe organic layer was dried over sodium sulfate
7. concentrationconcentrated under vacuum
8. customThe sample was purified by preparative TLC
9. washeluting with 7% methanol in dichloromethane which