反应详情

温度

0 °C

A solution of 1-(3-bromo-1-methyl-1H-1,2,4-triazol-5-yl)ethanol (1.639 g, 7.95 mmol, Eq: 1.00) and pyridine (944 mg, 965 μl, 11.9 mmol, Eq: 1.5) in dichloromethane (237 ml) was cooled to 0° C. then Dess-Martin periodinane (15% in dichloromethane, 24.7 g, 8.75 mmol, Eq: 1.1) was added. The resulting mixture was stirred for 4 hours at 0° C. under nitrogen atmosphere. The mixture was diluted with dichloromethane and washed with sat. sodium hydrogen carbonate. The organic layer was separated, dried over magnesium sulfate, filtrated and evaporated. The crude material was applied on silica gel and purified by flash chromatography over a 20 g silica gel column using dichloromethane/methanol 0-3% & 5% NH3 as eluent affording 1-(5-bromo-2-methyl-2H-[1,2,4]triazol-3-yl)-ethanone (948 mg, 58.4%) as a white solid. MS: m/z=203 (EI)

1. washwashed with sat. sodium hydrogen carbonate
2. customThe organic layer was separated
3. dry with materialdried over magnesium sulfate
4. filtrationfiltrated
5. customevaporated
6. custompurified by flash chromatography over a 20 g silica gel column