反应详情

To a solution of 3-(1,2,4-triazol-1-yl)propan-1-ol (7 g, 55 mmol) in DMF (70 ml) was added tertbutyldimethylsilyl chloride (9.1 g, 60 mmol) followed by DMAP (336 mg, 2.7 mmol) followed by imidazole (4.5gr, 66 mmol). After stirring overnight at ambient temperature, the volatiles were removed under vacuum and the residue was partitioned between water and ethyl acetate/ether. The organic layer was separated, washed with water, brine, dried (MgSO4) and evaporated. The residue was purified by column chromatography eluting with methylene chloride/ether (6/4) to give 3-(tertbutyldimethylsilyloxy)-1-(1,2,4-triazol-1-yl)propane (11.1 gr, 84%).

1. customthe volatiles were removed under vacuum
2. customthe residue was partitioned between water and ethyl acetate/ether
3. customThe organic layer was separated
4. washwashed with water, brine
5. dry with materialdried (MgSO4)
6. customevaporated
7. customThe residue was purified by column chromatography
8. washeluting with methylene chloride/ether (6/4)