反应详情

A solution of 1,2,3-thiadiazol-4-ylmethanol (0.75 g, 6.5 mmol) in dichloromethane (20 mL) was cooled to 5° C. under a nitrogen atmosphere and treated with triethylamine (1.018 mL, 7.3 mmol) and methanesulfonyl chloride (0.565 mL, 7.3 mmol). After 15 min, the ice-bath was removed and the reaction mixture was stirred for 2 h. The solution was washed with 1N hydrochloric acid solution (2×2 mL) and water, dried (MgSO4 +MgO) and concentrated. The residue was purified by chromatography (silica gel column 1.5×21 cm) with ether as eluting solvent to give 0.90 g (71%) of 1,2,3-thiadiazol-4-ylmethanol methanesulfonate;

1. customthe ice-bath was removed
2. washThe solution was washed with 1N hydrochloric acid solution (2×2 mL) and water
3. dry with materialdried (MgSO4 +MgO)
4. concentrationconcentrated
5. customThe residue was purified by chromatography (silica gel column 1.5×21 cm) with ether
6. washas eluting solvent