反应详情

To a solution of ammonium fluoride (10.4 g, 280 mmol) in methanol (110 ml) was added a solution of 3-(tertbutyldimethylsilyloxy)-1-(5-methyl-[1,2,4]-triazol-1-yl)propane (7.2 g, 28 mmol) in methanol (30 ml). The mixture was refluxed for 4.5 hours. After cooling, silica (100 g) was added and the volatiles were removed under vacuum. The residue was added onto a column of silica and eluted with a mixture of methylene chloride/ethyl acetate (1/1) followed by methylene chloride/methanol (9/1) to give 3-(5-methyl-[1,2,4]-triazol-1-yl)propan-1-ol (3.65 g, 92%).

1. temperatureThe mixture was refluxed for 4.5 hours
2. temperatureAfter cooling
3. additionsilica (100 g) was added
4. customthe volatiles were removed under vacuum
5. additionThe residue was added onto a column of silica
6. washeluted with a mixture of methylene chloride/ethyl acetate (1/1)